Ultrasound Assisted Extraction of Food and Natural Products. Mechanisms, Techniques, Combinations, Protocols and Applications. A Review

Ultrasonics Sonochemistry 34 (2017) 540560
Contents lists available at ScienceDirect
Ultrasonics Sonochemistry
journal homepage: www.elsevier.com/locate/ultson
Review
Ultrasound assisted extraction of food and natural products.

Mechanisms, techniques, combinations, protocols and applications.
A review
Farid Chemat , Natacha Rombaut, Anne-Galle Sicaire, Alice Meullemiestre, Anne-Sylvie Fabiano-Tixier,
Maryline Abert-Vian
Universit dAvignon et des Pays de Vaucluse, INRA, UMR408, GREEN Team Extraction, F-84000 Avignon, France
a r t i c l e i n f o a b s t r a c t
Article history: This review presents a complete picture of current knowledge on ultrasound-assisted extraction (UAE) in
Received 4 April 2016 food ingredients and products, nutraceutics, cosmetic, pharmaceutical and bioenergy applications. It pro-
Received in revised form 9 June 2016 vides the necessary theoretical background and some details about extraction by ultrasound, the tech-
Accepted 23 June 2016
niques and their combinations, the mechanisms (fragmentation, erosion, capillarity, detexturation, and
Available online 23 June 2016
sonoporation), applications from laboratory to industry, security, and environmental impacts. In addition,
the ultrasound extraction procedures and the important parameters influencing its performance are also
Keywords:
included, together with the advantages and the drawbacks of each UAE techniques. Ultrasound-assisted
Ultrasound-assisted extraction
Mechanisms
extraction is a research topic, which affects several fields of modern plant-based chemistry. All the
Hybrid techniques reported applications have shown that ultrasound-assisted extraction is a green and economically viable
Safety and security alternative to conventional techniques for food and natural products. The main benefits are decrease of
Green impacts extraction and processing time, the amount of energy and solvents used, unit operations, and CO2
Industrial application emissions.
2016 Elsevier B.V. All rights reserved.
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
2. Extraction mechanisms induced by ultrasound . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
2.1. Fragmentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 542
2.2. Erosion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 542
2.3. Sonocapillary effect . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 544
2.4. Sonoporation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 544
2.5. Local shear stress . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 544
2.6. Detexturation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 545
2.7. Combined mechanisms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546
3. Influencing parameters of ultrasound assisted extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546
3.1. Physical parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
3.1.1. Impact of ultrasound physical characteristics: power and frequency . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
3.1.2. Intensity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
3.1.3. Shape and size of ultrasonic reactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
3.2. Medium parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
3.2.1. Solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
3.2.2. Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
3.2.3. Presence of dissolved gases and external pressure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
3.2.4. Matrix parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
Corresponding author.
E-mail address: [email protected] (F. Chemat).
http://dx.doi.org/10.1016/j.ultsonch.2016.06.035
1350-4177/ 2016 Elsevier B.V. All rights reserved.
F. Chemat et al. / Ultrasonics Sonochemistry 34 (2017) 540560 541
4. Ultrasound techniques for extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548

4.1. Conventional techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
4.2. Hybrid techniques: combination of ultrasound with conventional methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 549
4.2.1. Sono-soxhlet: ultrasound assisted soxhlet extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 549
4.2.2. Sono-clevenger: ultrasound assisted clevenger distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
4.3. Combination of ultrasound with innovative techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 551
4.3.1. Combination of microwave and ultrasound . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 551
4.3.2. Combination of DIC process and ultrasound. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 551
4.3.3. Combination of ultrasound and supercritical fluid extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
4.3.4. Combination of ultrasound and extrusion extraction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
5. Protocols and applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
5.1. Fruits and vegetables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
5.2. Herbs and spices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 553
5.3. Oleaginous seeds . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 554
5.4. Microorganisms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 554
6. HACCP and HAZOP considerations using UAE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 555
7. Environmental impact of Ultrasound-assisted extraction (UAE) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 556
8. Up-scaling of UAE and its applications in industry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 556
9. Future trends . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 558
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 558
1. Introduction Ultrasound is a key-technology in achieving the objective of

sustainable green chemistry and extraction. Ultrasound is well
Extraction has been used probably since the discovery of fire. known to have a significant effect on the rate of various processes
Egyptians and Phoenicians, Jews and Arabs, Indians and Chinese, in the chemical and food industry. Using ultrasound, full extrac-
Greeks and Romans, and even Mayas and Aztecs, all possessed inno- tions can now be completed in minutes with high reproducibility,
vative extraction and distillation processes used even for perfumes, reducing the consumption of solvent, simplifying manipulation
cosmetics or food. Nowadays, we cannot find a production line in and work-up, giving higher purity of the final product, eliminating
food, pharmaceutical, cosmetic, nutraceutic, or bioenergy indus- post-treatment of waste water and consuming only a fraction of
tries, which do not use extraction processes, such as (maceration, the fossil energy normally needed for a conventional extraction
solvent extraction, steam or hydro-distillation, cold pressing, method such as Soxhlet extraction, maceration or Clevenger distil-
squeezing. . .). With the increasing energy costs and the drive to lation. Several classes of food components such as aromas, pig-
reduce greenhouse gas emissions, food and plant-based chemical ments, antioxidants, and other organic and mineral compounds
industries are challenged to find new technologies in order to reduce have been extracted, analyzed and formulated efficiently from a
energy consumption, to meet legal requirements on emissions, pro- variety of matrices (mainly animal tissues, microalgae, yeasts, food
duct/process safety and control, and for cost reduction and increased and plant materials).
quality as well as functionality. For example, existing extraction This review presents a complete picture of current knowledge
technologies have considerable technological and scientific on ultrasound-assisted extraction of food and natural products.
bottlenecks to overcome: often requiring up to 50% of investments The readers like chemists, biochemists, chemical engineers, physi-
in a new plant and more than 70% of total process energy used in cians, and food technologists even from academia or industry will
food industries [1]. In the last two decades, these shortcomings find a deep and complete perspective regarding ultrasound-
have led to the consideration of the use of enhanced and effi- assisted extraction. This review will not systematically address
cient extraction techniques amenable to automation such as the following topics, which were pertinently covered by recent
ultrasound-assisted extraction. Shorter extraction times, reduced reviews:
organic solvent consumption, energy and costs saved, were the main
tasks pursued. Driven by these goals, advances in ultrasound- Ultrasound cavitation theory [4];
assisted extraction have resulted in a number of innovative techniques Guidelines of good practice for UAE [5];
such as ultrasound-assisted Soxhlet extraction, ultrasound-assisted Application of ultrasound in food processing [6].
Clevenger distillation, continuous ultrasound-assisted extraction, and
combination of ultrasound with other techniques such as microwave, The first part presents the different mechanisms involved dur-
extrusion, and supercritical fluid extraction. ing UAE (fragmentation, erosion, capillarity, detexturation, and
To meet the requirements of the market and of the regulations, sonoporation) and influencing parameters. The second part is ded-
the sono-extract must meet a number of quality criteria, contrary icated to the importance of the ultrasound techniques and their
to some popular misconceptions; the natural state of the extract combinations. The third part focuses on applications of UAE in dif-
is no guarantee of its harmlessness to human and its environment. ferent fields and presentation of most relevant procedures. The last
In such changing context, nowadays we must include the change of part gives new insights in term of up-scaling and industrial appli-
extraction conscience from a simple interest in data analysis to cations, quality, security and safety considerations, environmental
interest in models and the strong consideration of the environmen- impacts and future directions for research and industry.
tal side effects of our practice as a consequence of the high demand
of extraction information. This evolution or revolution of extrac- 2. Extraction mechanisms induced by ultrasound
tion of natural products is resumed in Fig. 1. Green extraction of
naturals products could be a new concept to meet the challenges UAE of natural products has been widely investigated, with
of the 21st century, to protect both the environment and con- numerous examples, which could be found in literature. Addition-
sumers and in the meantime enhance competition of industries ally, a few very good reviews on the subject were published within
to be more ecologic, economic and innovative [2,3]. the last years [69]. However in these reviews and throughout
542 F. Chemat et al. / Ultrasonics Sonochemistry 34 (2017) 540560
Fig. 1. Ultrasound-assisted extraction: evolution or revolution.
literature, mechanisms leading to extraction enhancement due to chlorophyll extraction from spinach leaves (Fig. 2). This effect was
the use of ultrasound are rarely investigated. Some reference examined using an ultrasound probe (20 kHz, UIP1000 HdT,
papers describe the effects of ultrasound propagation in a solid/liq- Hielscher). During UAE, it was noticed a quick fragmentation of
uid media [10,11]. Cavitation phenomena leads to high shear forces the spinach leaves in the first minutes of sonication whereas leaves
in the media. The implosion of cavitation bubbles on a products did not seems impacted during conventional extraction performed
surface results in micro-jetting which generates several effects by maceration. The extraction kinetics of chlorophylls from spi-
such as surface peeling, erosion and particle breakdown. Addition- nach has been monitored by UV (Fig. 2-A). Comparing the extrac-
ally, implosion of cavitation bubbles in a liquid media leads to tion rate of chlorophylls between UAE process and maceration
macro-turbulences and to a micro mixing. Surprisingly, in most process, a linear increase is obtained at the beginning of UAE, cor-
publications dealing with UAE of natural products, the authors jus- responding to a direct solubilization of chlorophylls. This effect is
tify yields enhancement by cavitation effects occurring during most probably due to the reduction in particle size occurring dur-
ultrasonic irradiation without further investigations. ing application of ultrasound. Spinach residues were collected after
Toma et al. (2001) [12] demonstrated that a fragmentation of filtration to measure the particle size distribution (Fig. 2-B). On the
the matrix occurred during irradiation and an enhanced hydration chart are plotted particle size distributions below 1100 lm for resi-
of the matrix due to ultrasound. The authors also showed an dues from UAE and maceration. It has been noted that 80% of the
increase of the extraction index for sonicated samples compared sample mass for maceration particles are beyond 1100 lm and
to non-sonicated samples. To pursue the understanding and illus- could not be measured by the same equipment. The average parti-
trate the ultrasound effect on a vegetal matrix during UAE, we cle size of spinach residue after UAE (200 lm) is lower than the
examined closely different studies and we noticed that ultrasound maceration one (300 lm). Fragmentation of friable solids resulting
extraction doesnt act with one mechanism but through different from ultrasonic cavitation has been identified by several authors
independent or combined mechanisms between fragmentation, [11,13,14]. Fragmentation can be due to inter-particle collisions
erosion, capillarity, detexturation, and sonoporation. The following and from shockwaves created from collapsing cavitation bubbles
section aims at highlighting physical impacts of ultrasound on a in the liquid. A direct consequence of the reduction in particle size
vegetal matrix, which could be linked to extraction yield increase. by ultrasound action is the increase of surface area of the solid
All studies refer to high power ultrasound corresponding to fre- resulting in higher mass transfer and increased extraction rate
quencies of 20 or 25 kHz. and yield.
2.1. Fragmentation 2.2. Erosion
In some cases, during application of ultrasound in a liquid Some authors have already noticed erosion of raw plant mate-
media containing a raw material, it can be noticed a rapid fragmen- rial when treated by ultrasound. For example, UAE of boldo leaves
tation of the raw material. The impact of fragmentation induced by has been studied by Petigny et al. (2013) [15] using an ultrasonic
ultrasound is illustrated in this section throughout the example of probe (20 kHz, UIP1000 hd, Hielscher). Comparison of extraction
Fig. 2. Effect of power ultrasound on spinach leaves. (A: Comparison of chlorophyll extraction kinetics for UAE, US probe 20 kHz ( ) and for maceration (M, s);
B: Comparison of particle size repartition (below 1 mm) of spinach residue for UAE ( ) and for maceration (s)).
yields shows enhancement of extraction yield from 20% for con- surface of leaves, which seems to be specifically impacted by ultra-
ventional maceration to 25% with UAE (Fig. 3-A). Extraction rate sound (Fig. 3-B). Hence, theses structure seem to have been dam-
enhancement is also noted during the first stage of extraction. aged or removed from the leaf after ultrasound treatment, which
Comparison of SEM observations of leaf surface before and after is not the case of leaves submitted to maceration. The erosion
treatment show that leaves are not fragmented, but a localized enhanced accessibility of water as solvent to the leaf further
effect has been noticed. Boldo leaves possess trichomes on the improving extraction and solubilization. Given those observations,
Fig. 3. Effect of power ultrasound on boldo leaves. (A: Comparison of extraction kinetics of soluble matter in water for UAE, US probe 20 kHz ( ) and for maceration (s); B:
SEM microscopic observation of trichomes on leaf surface, 1) control leaf surface, 2) leaf surface after conventional process, 3) leaf surface after UAE; C: Proposed mechanism
for effect of cavitation bubbles on boldo leaf surface (a) Plant profile with a trichome at the surface of the leaf, (b) Generation of a cavitation bubble, (c) Collapse of the
cavitation bubble which generates a micro-jet directed towards the surface and (d) Abrasion of the surface, breaking of the trichome, and release of soluble material in the
surrounding medium).
a possible mechanism for extraction enhancement could be that directly acts on mass transfer improvement. The improvement of
implosion of cavitation bubbles on the leaves surface induces matrix WHC under ultrasound applied during meat brining or
erosion of plant structures released in the extraction medium meat curing has also been investigated by several authors
(Fig. 3-C). Erosion is a known effect of ultrasound and is used for [2529]. Authors reported a modification of meat structure after
several purposes such as cleaning or for sonochemical reactions an ultrasound treatment as well as enhancement of salt and mois-
e.g. with metals [16]. The study of Degrois et al., 1974 [17] had ture transfer using ultrasound processing. The parameter which is
already identified an erosion on starch granules produced by reported to have a key influence is ultrasonic intensity, where a
acoustic cavitation. Numerous pits are visible on the surface of threshold value for ultrasound influence could be identified
granules resulting from cavitation bubbles collapse. (e.g. between 40 and 50 W/cm2 for pork loins ultrasound assisted
brining [27]).
2.3. Sonocapillary effect
2.4. Sonoporation
The ultrasonic capillary effect (UCE) refers to the increase of
depth and velocity of penetration of liquid into canals and pores The sonoporation effect of ultrasound is well-known in the field
under some conditions of sonication [18,19]. This effect induced of biology and is applied when a permeability of cell membranes is
by ultrasound has recently been experimentally demonstrated desired. Sonoporation has been used in vitro for cell uptake in
for molten aluminum by Tzanakis et al., 2015 [20]. Although the molecules e.g. drugs, genes (reversible sonoporation) or for cell
mechanism for UCE is not fully understood, a relationship between destruction (irreversible sonoporation). For this, high ultrasound
cavitation and UCE has been established [21]. UCE could also be a frequencies are applied (beyond 500 kHz) [30,31]. However, a
mechanism explaining enhanced extraction performed under few studies focus on the use of low frequency (20 kHz) for cell wall
ultrasound. permeabilization [32] or bacteria inactivation [33].
In the study by Pingret et al., 2012 [22], recovery of total In the field of extraction, sonoporation can be used for reversi-
polyphenols from apple pomace was performed by ultrasound ble or irreversible cell membrane pores, which would result in
(Fig. 4-A). It can be identified that the extraction kinetics is release of cellular content in the extractive medium. Work
improved under ultrasound, although the major difference in the performed by our team on processing of wet yeast (Yarrowia
two extraction processes seems to be occurring in the first Lipolityca) for recovery of oil in yeast cells, has been studied by
10 min of extraction. We hypothesized that the difference could ultrasound at 20 kHz [34]. In Fig. 5, a comparison is made between
be due to a water absorption further favoring solvent access and untreated yeast (Fig. 5-A) and US-treated yeast (Fig. 5-B). Yeasts
diffusion of polyphenol out of the pomace. For this, we performed treated by ultrasound exhibit a highly impacted surface and perfo-
an additional experiment by measuring the Water Holding Capac- rations of the visible membrane have been noticed. Moreover,
ity (WHC) by a method described by Huang et al., 2016 [23] compared to conventional extraction without use of ultrasound, a
(Fig. 4-B). The method was adapted to only 10 min to assess the higher oil extraction yield has been obtained. Pore formation in
effect of solid/liquid mixing (maceration by agitation and US). the membrane caused by cavitation; hypothesis which is sup-
WHC is around 70% higher for ultrasound-treated pomace com- ported by the visualization of yeasts surface modification that
pared to maceration (Fig. 4-B). This observation confirms that could explain the higher yields reached.
water absorption is higher at the beginning of extraction and could
contribute to explain the increase extraction yield during the first 2.5. Local shear stress
part of extraction.
The impact of UCE on extraction was proposed by Vinatoru During irradiation of a solid-liquid mixture by ultrasound, some
(2001) [24]. The author also identified that the swelling index of shear forces are generated within the liquid and at the vicinity of
several vegetable matrix was increased from 5 to 10% by using solid materials. Shear forces and turbulences result from the evolu-
ultrasound and correlated this result to an increase of the extraction (oscillation and collapse) of cavitation bubble within the fluid.
tive value of the tested vegetables matrices. By increasing the Resulting streaming and acoustic micro-streaming effects are of
swelling and rehydration of a vegetable tissue, ultrasound impacts interest in applications such as mixing or emulsification [35].
positively on the basic mechanisms of extractions: desorption and Regarding UAE, shear effects could explain some observations
diffusion of a solute out of a vegetable structure. In this way, UCE previously made [36], where oil enrichment in basil essential oil
Fig. 4. Ultrasonic capillary effect induced by high power ultrasound on apple pomace. (A: Comparison of total polyphenol extraction (TPC) by maceration under agitation ( )
and by ultrasound (ultrasound reactor 1 L, 25 kHz, ambient temperature) ( ); B: Comparison of Water Holding Capacity of apple pomace after 10 min, for maceration under
agitation and ultrasound (US probe, 20 kHz, ambient temperature)).
Fig. 5. Effect of power ultrasound on Yarrowia Lipolityca (A: SEM microscopy for control yeast; B: SEM microscopy for US-treated yeast).
was investigated. Basil leaves were submitted to ultrasound in [38]. To assess this latter hypothesis, we compared the US power
olive oil (US reactor, 1L, REUS, ambient temperature). Extraction dissipation in olive oil and eugenol (Fig. 6-B). Temperature increase
kinetics of eugenol, a representative terpene contained in basil is higher with olive oil than with eugenol, which is due to a higher
essential oil is compared between UAE and maceration (Fig. 6-A). heat capacity for eugenol than for vegetable oil. Quantification of
For eugenol extraction by UAE a direct solubilization is noted, power dissipation (calculated according to Eq. (1)) is higher in
whereas the extraction process seems more diffusive in the case eugenol than olive oil, which would indicate that cavitation occur-
of maceration. In basil, essential oils are contained in glands which ring in essential oil could be more important than in olive oil.
are located at the surface of leaves (Fig. 6-C-1) [37]. For leaves trea-
ted by maceration in olive oil, the oil gland external envelop is still 2.6. Detexturation
intact (image 2). In the case of leaves observed after an ultrasound
irradiation, the oil gland seems to have exploded. It can be also In some cases after US extraction, a destruction or detexturation
noted that no other impact of ultrasound (e.g. pitting or erosion) of plant structures has been observed. This effect has been noticed
is visible on the leaf, aside from the oil gland. It could be hypothe- in a previous study on essential oil extraction from caraway seeds
sized that shear forces generated locally at the collapse of cavita- [39]. Total oil yields are similar between conventional extraction
tion bubble close to the oil gland could cause its rupture. (reflux extraction with hexane) and UAE (US probe, 20 kHz), how-
Another hypothesis could be that there is a pressure build-up ever a higher selectivity towards terpenes was noted for UAE
within the gland or occurrence of cavitation inside the gland itself (Fig. 7). Distinguishable physical modifications of caraways seeds
Fig. 6. Effect of power ultrasound on basil leaves. (A: Comparison of extraction kinetics of eugenol in olive oil for UAE, US reactor 25 kHz ( ) and for maceration (s); B: US
power dissipation during sonication for eugenol ( ) and olive oil (4); C: SEM microscopic observation of an essential oil gland, 1) control, 2) after maceration and 3) after UAE
(US reactor 25 kHz)).
Fig. 7. Effect of power ultrasound on carvi seeds. (SEM microscopy for untreated seeds (1), seeds after conventional extraction (2) and UAE: US probe, 20 kHz after 30 min, (3)
and after 60 min, (4)).
were noticed according to the extraction process used. Untreated succession of compression and rarefaction phases, which results in
seeds appear filled and intact. Observations of residual caraways a longitudinal displacement of those constitutive molecules. The
seeds after conventional extraction and UAE at low temperature molecules forming the liquid phase are temporarily dislodged from
enable to identify different modifications (Fig. 7). their original position and during the compression cycles, they can
Conventional extraction leaves the cells structures intact but collide with the surrounding molecules. During the rarefaction
emptied due to transfer of cell content in the solvent. A gradual phases, a negative pressure will be exerted, pulling the molecules
degradation of cell walls is obtained after ultrasound: at 30 min, apart [42]. The extent of the negative pressure depends on the nat-
cell walls are affected at various degrees and at 60 min of treat- ure and purity of the liquid [10,42]. At a sufficient high intensity of
ment, cells structures are totally broken and converted to unde- a sound wave, during a rarefaction phase the attraction forces
fined shapes (Fig. 7). It could be assumed that such cell between them might be exceeded, generating a cavity in the liquid
disruption favored accessibility to the solvent. Such destruction [10]. In a liquid, the cavities created into the medium are cavitation
or detexturation of cells structures is rarely reported after UAE, bubbles.
but some studies and reviews indicate a destructive effects on liv- The cavitation bubbles are able to grow by coalescence, and/or
ing cells and micro-organisms or enzymes [40]. rectified diffusion [43,44] since vapors or gas dissolved in the med-
ium will enter the bubble during rarefaction phase and will not
2.7. Combined mechanisms fully be expelled during the compression cycle. Cavitation bubbles
are commonly classified in to two types: stable and transient
Overall, several mechanisms have been identified as acting on [10,44]. Stable cavitation bubbles undergo many compression
ultrasound assisted extraction: fragmentation, erosion, sonocapil- and rarefaction cycles and oscillate often non-linearly around an
lary effect, sonoporation, local shear stress and destruction- equilibrium size. The transient cavitation bubbles exist for one or
detexturation of plant structures. Aiming at clarification, we chose at most for a few acoustic cycles, during which they expand very
to explicit and give evidence of each effect separately. However, quickly to at least double their initial size before collapsing vio-
during UAE a combination of effects most probably occurs. Also, lently into smaller bubbles [10,44]. Although transient cavitation
perhaps these effects are sequential during the extraction process. bubbles are considered as active cavitation bubbles, Ashokkumar
Additionally, although not detailed as a mechanism, the intense (2011) [43] highlighted that both types of bubbles are high-energy
mixing effect generated by the propagation of ultrasound in the collapse bubbles.
liquid medium contributes to enhancement of mass transfer, When the size of these bubbles reaches a critical value, they col-
greatly improving the solute transfer rate. The mixing effect at a lapse during a compression cycle and a transitory hot spot is cre-
macroscopic scale is due to acoustic streaming and at a local stage, ated [45]. The collapse of cavitation bubbles generates extreme
acoustic microstreaming occurs [35]. Combining mixing effects to local conditions: determined temperatures up to approximately
physical impacts of ultrasound on raw material may explain the 5000 K [45] and estimated pressures around 501000 atm [11].
enhanced extraction performances of ultrasound. Hotspots created are able to accelerate dramatically the chemical
Comprehension of the possible mechanisms also points out that reactivity of the medium [45,46].
raw material has the major impact on extraction. Additionally, the When acoustic cavitation bubbles collapse near and onto the
type of pretreatment applied on the raw material to be treated will surface of a solid material, a number of physical effects are
also contribute to extraction performances; e.g. milling, flaking, reported [11]. The collapse of the bubble generates high-speed jets
drying will affect the accessibility of the compounds to be of liquids into the surface and creates shockwave damages. Those
extracted. A future trend could to identify if a generalization of effects can lead to fragmentation of friable materials and localized
ultrasound effect depending on the type of raw material could be erosion. In the case of a solid-liquid slurry, the acoustic cavitation
obtained. and shockwaves induce intense macro-turbulence, micro-mixing
and subsequently interparticle collisions. It results from these fac-
3. Influencing parameters of ultrasound assisted extraction tors an overall enhanced reactivity in the media and an increased
mass transfer of solid particles due to reduction of particle size.
Sonochemical effects of ultrasound in a liquid are attributed to In this section, those parameters, which influence Ultrasound-
the acoustic cavitation phenomena [11]. In the ultrasound field, Assisted Extraction (UAE), are detailed. The study of those parame-
acoustic cavitation generally refers to bubble formation, growth ters is of great importance in order to obtain a high extraction
and implosion occurring during the propagation of an ultrasound efficacy often resulting in obtaining the highest extraction yield.
wave in a liquid media [41]. The molecules constitutive of the liq- However, it is necessary to consider that the yield is not always
uid medium are held together by attractive forces [42]. The propa- the sole objective of an extraction process, but also the lowest use
gation of an ultrasound wave through an elastic medium induces a of non-renewable resources along with low energy consumption.
3.1. Physical parameters frequencies (500 kHz) compared to 20 kHz. Interestingly, Chuk-
wumah et al. (2009) [58] report a selective extraction of some phe-
As ultrasound is a mechanical wave, its characteristics such as nolics from peanuts according to the frequency applied: at 25 kHz
frequency, wavelength and amplitude can influence the acoustic (higher extraction of daidzein and genistein) and 80 kHz (biocha-
cavitation and therefore extraction. The influence of power input nin A and trans-resveratrol). However, longer extraction durations
as well as the reactor design and shape of the probe can influence where required when using the 80 kHz frequency. Gonzlez-
the process [47]. The impact of those parameters will be reviewed Centeno et al. (2014) [59] evaluated three frequencies (40 kHz,
in this section. 80 kHz and 120 kHz) for the extraction of phenolics from grape
pomace. Using the response surface methodology for the study of
3.1.1. Impact of ultrasound physical characteristics: power and influencing parameters, the authors highlighted that 40 kHz was
frequency most effective.
The measurement of the actual applied acoustic power in a As ultrasound frequency increases, the production and intensity
sonochemical process is not always reported, although some phys- of cavitation in liquid decreases [10]. At high frequency, the acous-
ical methods, which allow the direct or indirect measurement of tic cavitation would be more difficult to induce since the cavitation
the applied energy, are available. These methods estimate the bubbles need a delay to be initiated during the rarefaction cycle
transferred energy by measuring either chemical or physical and cycles of compression-rarefaction can be too short to allow
changes on the medium when ultrasound is applied. The most the increasing growth of the cavitation bubbles. The length of rar-
common physical methods are the measurement of acoustic pres- efaction phase (during which cavitation bubbles grow) is inversely
sure using hydrophones or optical microscopes, the aluminum foil proportional to ultrasonic frequency; therefore at high frequencies,
method and the calorimetric method [4850]. And among the larger amplitudes and intensities are required to generate cavita-
chemical methods, the indirect measurement of OH radicals tion [10].
formed by sonoluminescence or chemical dosimeters are also used At low frequencies, the transient cavitation bubbles are rela-
[51,52]. As an example, to calculate the power by calorimetry, it is tively less numerous although with high diameter, which privi-
considered that the actual input power from the device is con- leges the physical effects instead of the chemical ones [44,60].
verted to heat which is dissipated in the medium. In this case, The effect of the frequency may be linked not only to the cavitation
the effective ultrasound power is calculated according to Eq. (1) bubble size, but also to its influence on the resistance to mass
[53,54]. transfer [61].
dT 3.1.2. Intensity
P m:Cp: 1
dt Ultrasonic intensity is expressed as the energy transmitted per
second and per square meter of emitting surface [8]. This parame-
where Cp is the heat capacity of the solvent at constant pressure
ter is directly correlated to the amplitude of the transducer and
(J.g1.C1), m is the mass of solvent (g) and dT/dt is the tempera-
consequently to the pressure amplitude of sound wave [62]. With
ture rise per second.
the increase in the pressure amplitude, bubble collapse will be
Several studies show that high ultrasonic power causes major
more violent. To achieve cavitation threshold, a minimum value
alterations in materials by inducing greater shear forces (depend-
of UI is required. Regarding extraction, determination of ultrasonic
ing on the nature and properties of the medium); however, in
intensity (UI) is a relevant input value impacting strongly on
the food industry this parameter is usually optimized in order to
extraction efficiency. UI is calculated using the calculated power
use the minimum power to achieve the best results [55]. Generally,
delivered to the media as shown in Eq. (2) [8].
the highest efficiency of UAE, in terms of yield and composition of
the extracts, can be achieved by increasing the ultrasound power, P
UI 2
reducing the moisture of food matrices to enhance solvent-solid S
contact, and optimizing the temperature to allow a shorter extrac-
where UI is the ultrasonic intensity (W/cm2), P is the ultrasound
tion time. However, some studies showed the power variation can
power (W) as calculated by the Eq. (2), and S is the emitting surface
result in a certain selectivity of target molecules, where the ratio of
of the transducer.
some molecules is a function of the applied power [39,56]. US fre-
The increase of UI generally results in an increase of sonochem-
quency may also impact on the extraction process and have to be
ical effects [10]. As increasing the amplitude can increase UI, it is
chosen. The frequency will impact on the bubble resonance size.
important to note that high amplitudes can lead to rapid deteriora-
For example, the bubble characteristics are compared at 20 kHz
tion of the ultrasonic transducer, which results in liquid agitation
and 500 kHz in Table 1.
instead of cavitation and in poor transmission of the ultrasound
The most commonly used frequencies in UAE processes are
through the liquid media. However, the amplitude should be
comprised between 20 kHz and 100 kHz. The use of higher fre-
increased when working with high viscosity liquids such as oils
quencies for ultrasound assisted extraction has been investigated
[62].
in only few studies. Toma et al. (2001) [12] noticed a reduced phys-
Effect UI was evaluated at 16.4, 20.9 and 47.6 W/cm2 at 20 kHz
ical impact on the structure of marigold petals when applying high
for soybean oil extraction [63]. The study shows an increase in
yield up to 20.9 W/cm2, beyond which no further increase is noted.
Table 1 A similar tendency was noted by Wang et al. (2015) [64], which
Comparison of characteristic values at 20 kHz and 500 kHz for air saturated water at study on UAE of pectin at 20 kHz indicate that UI (varied between
an ultrasonic intensity of 10 W/cm2 (from Ptrier et al., 2008 [57]). 10.18 and 14.26 W/cm2) should be subjected to an optimization,
Frequency Amplitude Acoustic Wavelength Collapse Average since the highest value of UI not leading to the highest yields.
pressure duration diameter of Therefore it seems that UI is a parameter that should be studied
pulsating for optimization of UAE.
bubble
(kHz) (lm) (atm) (cm) (ls) (lm)
3.1.3. Shape and size of ultrasonic reactors
20 2.95 5.4 7.42 10 330
500 1.1 5.4 0.29 0.4 13
Since ultrasound waves are reflected when a solid surface is
attained, in the case of extraction using an ultrasonic bath, the
shape of the reaction vessel is critical. The best choice would be a cavitation bubbles may be reduced. Therefore, sonochemical
flat bottom vessel such as a conical flask in order to attain a min- effects are favored by low temperatures and a control of tempera-
imum reflection of waves [65]. The thickness of the vessel should ture is usually applied to limit temperature rise [70].
also be kept to the minimal to reduce attenuation [62]. It is neces- For extraction processes, temperature contributes to efficiency
sary to calculate the optimum reactor dimensions and the position of extraction. Usually, increase of temperature leads to an increase
of the emitter in relation to the transducer to attain maximum of extraction yield [71]. In the case of UAE, some authors report a
energy transferred to the medium [66]. Further advances have beneficial effect of temperature rise from 20 C to 70 C compared
been made by taking into account the lack of homogeneity of the to non-sonicated extractions [7]. This effect has been justified by
pressure field in the reactor in order to optimize the process effi- an increase in the number of cavitation bubbles and a larger
ciency [61,67]. Also, in the case of ultrasonic probes a rapid solid-solvent contact area, enhancements of solvent diffusivity
decrease of intensity is observed both radially and axially. For with consequent enhancement of desorption and solubility of the
this reason a minimal space between the ultrasonic probe and interest compounds. However, this effect is decreased when the
the wall of the container must be respected, while ensuring that temperature is near the solvents boiling point and most authors
the probe does not touch the container to avoid damages on the report a beneficial effect of low temperature (below 30 C) in the
material [62]. case of UAE [61,72,73]. It is important to choose an extraction tem-
In the case of the use of an ultrasonic probe, the shape and perature according to the target compound of extraction [74,75].
diameter of this last one may have an influence on the extraction. Hence, a temperature control is necessary to prevent the degrada-
The stepped probe gives the highest amplitude magnification tion of thermolabile compounds. The optimization of temperature
(i.e., power, amplitude gain (D/d)2) of the shapes shown. Neverthe- parameter can be performed in order to obtain the highest yield of
less, the exponential probe shape offers small diameters at its the target compounds without degradation, since this parameter
working end, which makes it particularly suited to micro- can vary depending on the type of product.
applications [62].
Most of the probe emitters are composed of a titanium alloy, 3.2.3. Presence of dissolved gases and external pressure
since this material is thermo-resistant and behaves well under cor- The absence of gases renders formation of cavitation bubbles
rosive conditions. However, the erosion of this material is often difficult, since cavitation bubbles are formed from gas (vapors) dis-
important, leading to transfer of metal particles into the extraction solved in the liquid [57]. Dissolved gases into the solvent act as
medium. Some new materials are investigated for ultrasound nuclei for a new cavitation bubble [10,44]. However, application
probe tips, such as quartz and Pyrex, which might solve the prob- of ultrasound tends to degas a liquid. A gas bubbling can be used
lem of metal particles release [68]. to control composition of cavitation bubbles and can affect sono-
chemical effects [10]. Generally, in the field of extraction, the com-
3.2. Medium parameters position of gases dissolved in the solvent is not controlled.
If external pressure is increased, then a greater acoustic pres-
The medium presents intrinsic characteristics that need to be sure is required to induce cavitation. But once the cavitation
taken into consideration in order to achieve the expected results threshold is reached under external pressure (>1 atm), the inten-
in the extraction process assisted by ultrasound. sity of the cavitation bubble collapse is higher than without pres-
sure and consequently, an enhancement in sonochemical effects
3.2.1. Solvent is obtained [44,62].
Solvent choice in UAE is driven by the solubility of the target
metabolites but also by physical parameters such as viscosity, sur- 3.2.4. Matrix parameters
face tension and vapor pressure of the solvent. Those physical Depending on the objective of the UAE and the target mole-
parameters will affect the acoustic cavitation phenomenon and cules, plant matrix could be used either fresh (e.g. algae, yeast. . .)
more specifically cavitation threshold [10]. The initiation of cavita- or dry (e.g. herbs, oleaginous seeds. . .). The pre-treatment of the
tion in a liquid requires that the negative pressure during the rar- matrix is important and can impact extraction efficiency [24].
efaction cycle have to overcome the cohesive forces between The solubility and stability of the target compounds in the chosen
molecules composing the liquid. A rise of viscosity, or a rise of sur- solvent and temperature of the liquid medium can influence the
face tension, induces an increase of these molecular interactions final yield of the extraction. Likewise, since the extractive system
hence raising significantly the cavitation threshold. In this manner, is a heterogeneous and complex porous media, the size of the cav-
the amplitude should be increased when working with samples of itation bubble has an effect on the efficiency on the extraction.
high viscosity. This is because as the viscosity of the sample Other parameters related to the solid-liquid extraction such as
increases so does the resistance of the sample to the movement the solid/liquid ratio and particle size of the material are relevant
of the ultrasonic device, for instance the tip of an ultrasonic probe. to the efficacy of extraction. The extraction yields may vary also
Therefore, a high intensity (or high amplitude) is advised in order due to plant materials structure, plasticity or compositional differ-
to obtain the necessary mechanical vibrations that will result in ences which will result in different degrees of impacts from cavita-
cavitation [62]. A solvent with low vapor pressure is preferred in tion effects [35].
UAE, as the collapse of cavitation bubble is more intense compared
to solvents with high vapor pressure [69]. However, vapor pressure 4. Ultrasound techniques for extraction
depends on the temperature in the liquid medium.
4.1. Conventional techniques
3.2.2. Temperature
The temperature strongly impacts the solvents properties. An High power ultrasound can be applied using two types of
increase of temperature results in a decrease of both viscosity devices, ultrasonic bath or probe-type ultrasound equipment. Both
and surface tension, and induces an increase of vapor pressure. A systems are based on a transducer as a source of ultrasound power.
rise in vapor pressure causes more solvent vapors to enter the bub- The piezoelectric transducer is the most common type used in the
ble cavity and numerous cavitation bubbles, which will collapse majority of ultrasonic reactors. The ultrasonic bath is the most
less violently and reduce sonication effects [62]. As a consequence, commonly known type of ultrasonic device usually consists of a
at higher temperatures, the sonochemical effects due to collapse of stainless steel tank with one or more ultrasonic transducers.
Ultrasonic baths usually operate at a frequency of around 40 kHz system to the liquid media induces a quick increase of temperature
and can be equipped with temperature control. They are readily in the reactor. The cooling of the reactor by a double-jacket is then
cheap, available and large numbers of samples can be simultane- required to conduct extraction. The manufacturers of high-power
ously treated. However, compared with probe systems, the low ultrasound equipment have been focusing on designing devices
reproducibility and low power of ultrasound delivered directly to which include specific operational features such as continuous
the sample are major drawbacks. Indeed, the delivered intensity flow mode. The equipment basically consists of a glass or stainless
is highly attenuated by the water contained in the bath and the steel reactor, through which the fluid mixture is pumped at atmo-
glassware used for the experiment. Recently a new bath system spheric or high pressure to conduct mano-sonication. The continu-
reactor has been developed by REUS (Contes, France) operating ous reactor could be cooled or heated with a double mantle to
at 25 kHz, which is mostly used for extraction applications. It con- conduct mano-thermo-sonication (D, Fig. 8).
sists in a stainless steel reactor equipped with a double-layered
mantle with water circulation to allow temperature control with 4.2. Hybrid techniques: combination of ultrasound with conventional
cooling/heating systems. methods
High power ultrasonic probes are generally preferred for extrac-
tion applications. The probe system is more powerful due to an 4.2.1. Sono-soxhlet: ultrasound assisted soxhlet extraction
ultrasonic intensity delivered through a smaller surface (only the Fats and oils are traditionally extracted from their matrix using
tip of the probe), when comparing to the ultrasonic bath. They the Soxhlet extraction. Invented in 1879, this apparatus has been
are generally operated at around 20 kHz and use transducer widely used in various fields such as environmental applications,
bonded to probe which is immersed into the reactor resulting in foodstuffs and also pharmaceutics. Its principle is relatively easy
a direct delivery of ultrasound in the extraction media with mini- and proceeds by an iterative percolation of condensed vapors of
mal ultrasonic energy loss. There are several designs of probes with a boiled solvent, generally n-hexane. Nevertheless, Soxhlet extrac-
different lengths, diameters and tip geometries. The probe selec- tion has some disadvantages such as a long operation time (several
tion is made according to the application and to the sample volume hours), large solvent volumes, evaporation and a concentration
to be sonicated. The intensity of ultrasound delivered by the probe step needed at the end of the extraction. There are only few
Fig. 8. Commonly used ultrasonic systems (A: Ultrasound bath, B: Ultrasound reactor with stirring, C: Ultrasound probe, D: Continuous sonication with ultrasound probe).
processes in the literature that have reported the combination of 6 to 24 hours. During distillation, fragrant plants exposed to boiling
Soxhlet extraction with innovative techniques, such as ultrasound, water or steam, release their essential oils through evaporation.
for the acceleration of fat and oil extraction. Recovery of the essential oil is facilitated by distillation of two
The teams of Luque de Castro and Chemat [76,77] developed immiscible liquids, namely, water and the essential oil. This is
original Sono-Soxhlet methods. Ultrasound is applied outside or based on the principle that, at the boiling temperature, the com-
inside the extraction chamber to enhance the solid liquid extrac- bined vapor pressures equal the ambient pressure. Thus the essen-
tion and migration of metabolites from solid matrix to solvent tial oil ingredients, for which boiling points normally range from
(Fig. 9 a and b). Sono-Soxhlet combines the advantages of the 200 to 300 C, are evaporated at a temperature close to that of
extraction performed with Soxhlet (extraction repeated by a fresh water. As steam and essential oil vapors are condensed, both are
solvent) and enhancing mass transfer with ultrasound (reduction collected and separated in a vessel traditionally called the Floren-
of extraction time). The process ensures the complete, rapid and tine flask". The essential oil, being lighter than water, floats at the
accurate extraction of the samples. This system has been also been top while water goes to the bottom and is separated.
used for the extraction of the oil content and the fatty acid compo- With growing a flavour and fragrance industry and the increas-
sition of oleaginous seeds, lipids from sausage products, fat from ing demand for more natural products, the need for novel extrac-
cheese and bakery products. tion methods has become more intense. The combination of
ultrasound with Clevenger or alembic distillation has attracted
4.2.2. Sono-clevenger: ultrasound assisted clevenger distillation growing interest in the past few years. This has resulted in the
The traditional method used to isolate volatile compounds as development of Sono-Clevenger [78] specifically aimed for obtain-
essential oils from plant material (herbs, spices, barks, fruits. . .) ing essential oils from plant materials. Sono-Clevenger is an origi-
is alembic distillation that, in chemistry laboratories, is also called nal combination of ultrasound cavitation and Clevenger distillation
Clevenger distillation. This method proceeds by the iterative distil- at atmospheric or reduced pressure (Fig. 9 c and d). It provides
lation and boiling of the aromatic matrix, it generally uses large yields comparable to those obtained by traditional hydrodistilla-
quantities of water and energy. The extraction time can vary from tion but with reduced extraction times and enhanced yields. The
Fig. 9. Hybrid extraction techniques ((a) conventional Soxhlet, (b) Sono-Soxhlet, (c) conventional Clevenger, (d) Sono-Clevenger).
thermally sensitive crude materials seem to be preserved with this of the material can be irreversibly damaged. This is however a
method, in contrast to conventional Clevenger distillation. minor limitation because UMAE requires lower power levels than
the two single energy sources alone. Ultrasound can dramatically
4.3. Combination of ultrasound with innovative techniques improve the extraction of a target component mainly through
the phenomenon of cavitation. The mechanical ultrasonic effect
4.3.1. Combination of microwave and ultrasound promotes the release of soluble compounds from the plant body
The combination of ultrasound-assisted extraction (UAE) and by disrupting cell walls, enhancing mass transfer and facilitating
microwave-assisted extraction (MAE) by means of simultaneous solvent access to cell content. Meanwhile, MW heats the whole
irradiation (UMAE) is one of the most promising hybrid techniques sample very quickly inducing the migration of dissolved molecules.
for fast, efficient extractions. Since the pioneering work of Cravotto The simultaneous irradiation increases solvent penetration into the
et al. [68], several applications of combined US/MW irradiation for matrix, facilitates analyte solvation and usually increases the solu-
plant extraction have appeared in the literature, the great potential bility of target compounds.
of this hybrid technique has not yet been adequately exploited UMAE has been successfully employed by Cravotto and Binello
(Fig. 10 a). Due to the high efficiency and the dramatically short [80] as a complementary technique in the extraction of oils from
extraction time, we believe that UMAE has a great potential for vegetable sources; viz., soybean germ and a cultivated seaweed
academic and industrial research activity. It is a cost-effective rich in docosahexaenoic acid (DHA).
extraction technique for fast sample preparation and a new strat-
egy for process intensification. If, on one hand, double simultane- 4.3.2. Combination of DIC process and ultrasound
ous irradiation can bring additive or even synergic effects to the The Instantaneous Controlled Pressure Drop process, abbrevi-
extraction phenomenon of vegetal matrices, on the other, non- ated DIC according to the French expression Dtente Instantane
metallic horns can only be used at moderate power. As described Contrle. DIC extraction is based on fundamental studies con-
by Cravotto and Cintas [79], Pyrex, quartz or Peek made horns cerning the thermodynamics of instantaneity. It involves a
can be safely used up to 90 W, above that the intrinsic structure thermo-mechanical processing induced by subjecting the product
Fig. 10. Combined innovative extraction techniques ((a) ultrasound-microwave, (b) ultrasound DIC, (c) ultrasound-SFE, (d) ultrasound-extrusion).
to a fast transition from high steam pressure to vacuum. DIC 4.3.4. Combination of ultrasound and extrusion extraction
extraction usually starts by creating a vacuum condition, followed For the production of sugar, wine and fruit juices, or the dehy-
by injecting steam into the material for several seconds, proceed- dration of biological wastes and in vegetables oil industries, extrac-
ing then to a sudden pressure drop towards vacuum (about 5 kPa tion is realized by pressing and extrusion. The pressing phase is
with at a rate higher than 0.5 MPa/s). By suddenly reducing the composed of a compression step to exude a fluid containing the
pressure, rapid auto-vaporization of the moisture inside the mate- target metabolites from the porous matrix. The cells of fruit and
rial will occur. It will swell and lead to texture change, which vegetable tissues are surrounded with membranes and closed by
results in higher porosity as well as increased specific surface area a cell wall embedded into a middle lamella. The rigid wall compo-
and reduced diffusion resistance. nents prevent easy damage of the membranes, and thus limit effi-
The combination of these two innovative techniques, cavitation ciency of the pressing extraction. The combination of pressing with
(US) and mechanical (DIC), and their application to physical pro- other processes such as ultrasound can be studied in a research
cesses like extraction appears to be interesting (Fig. 10 b). How- context, in order to obtain better extracts (quality and quantity
ever, it is not known how simultaneous US-DIC action could versus time) at the stage of process intensification (Fig. 10 d). In
bring about a physical effect. Therefore, it is expected that the general, the average extrusion force decreases with an increase
kinetics of the extraction processes will improve, but also it is in ultrasound amplitude resulting in better extrudability [83,84].
thought that a new effect may occur. For instance, the high pres-
sure level induced by DIC and the difference between internal
and external pressure (controlled by Darcy law) could induce par- 5. Protocols and applications
ticle fragmentation and exudation, and ultrasound cavitation could
induce fragmentation and erosion of solid particles and also induce 5.1. Fruits and vegetables
enhanced mass transfer from the inside to the outside of the trea-
ted matrix. A combination of DIC (pressure phenomena) and ultra- Fruits and vegetables are frequently used for the extraction of
sound (cavitation) has been successfully applied to extraction with various molecules of interest such as antioxidants, pigments, lipids,
yield enhancements and a reduction in treatment time [81]. The phytochemicals and aromas, intended for direct or indirect appli-
sequential use of DIC and ultrasound assisted extraction triggered cations in food, pharmaceutical and cosmetic industries. Fruits
complementary actions materialized by supplementary effects. and vegetables contain a wide range of secondary metabolites in
These effects can be illustrated through an example where sequen- pulp, peel, seeds, and bark. Table 2 presents some applications of
tial extraction of essential oil and antioxidants was made. the use of ultrasound for the extraction of different kind of com-
The impact of process combination on extraction was evaluated pounds from various fruits and vegetables. Antioxidants are able
by comparison to two standard processes: hydrodistillation (HD) to prevent the oxidation process by reacting preferably with oxi-
and solvent extraction (SE). First, the extraction of orange peel dizing agent instead of the target cells or molecules of interest
Essential Oil (EO) was achieved by HD during 4 h and DIC process [85]. Nowadays, there is a need in cosmetic, pharmaceutical and
(after optimization) during 2 min; EO yields was 1.97 mg/g dry food industries to replace synthetic substances such as butylated
material (dm) with HD compared to 16.57 mg/g dm with DIC. In hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) which
the second part of the study, the solid residue was recovered to have shown some negative side effects on health [86]. Isolation and
extract antioxidant compounds (naringin and hesperidin) by SE purification of natural antioxidants from natural plants is a critical
and UAE. Scanning electron microscopy of the residues showed step due to the co-extraction of undesirable by-products such as
that, after HD the recovered solid shriveled as opposite to DIC pigments, oils, waxes from matrices.
treatment which expanded the product structure. After 1 h of Conventional techniques for antioxidants extraction are macer-
extraction, DIC treated orange peels with UAE extracts contained ation and Soxhlet extraction, which are time-consuming and
0.825 0.016 g/g of dm for hesperidin and 0.0645 0.0002 g/g dm require large volume of solvent [87]. Pan et al. [88] have reported
for naringin compared to 0.640 0.027 g/g dm and 0.057 a comparison between UAE and conventional extraction of antiox-
0.002 g/g dm, respectively with SE. By combining DIC to UAE, idants from pomegranate peel. For the both extraction processes,
it was possible to enhance kinetics and yields of antioxidant pomegranate marc was obtained after the juice processing of
extraction. pomegranate fruit, then dried at 40 C and ground using a hammer
mill to achieve a particle size less than 40-mesh. Conventional
maceration was performed using a water/peel ratio of 50/1
4.3.3. Combination of ultrasound and supercritical fluid extraction (w/w). Maceration was done with agitation (magnetic stirring at
Supercritical fluid extraction (SFE) is a relatively recent extrac- 1200 rpm) and was performed following a kinetic of extraction of
tion technique based on the enhanced solvent power of fluids 290 min at room temperature. Concerning UAE, ultrasound probe
above their critical point. Its usefulness in extractions is due to with area of 1.267 cm2 and intensity levels between 2.4 and
the combination of gas-like mass transfer properties and liquid- 59.2 W/cm2 was used at constant frequency of 20 kHz. The sample
like solvating characteristics with diffusion coefficients, which container was kept constant at 25 C, and covered by an
are higher than those of a liquid. The majority of SFE studies have aluminum-foil paper to prevent photo-oxidation. The perfor-
focused on the use of CO2 because it is non-toxic, non-flammable, mances of UAE were performed in continuous and pulsed modes
cheap, easily eliminated after extraction and endowed with a high with total extraction times of 2, 10, 20, 30, 60, and 90 min, as being
solvating capacity for non-polar molecules. The major advantages during conventional extraction. The optimal condition obtained for
of SFE include pre-concentration effects, cleanness and safety, UAE was 59.2 W/cm2 for intensity level and an extraction time of
higher yields, expeditiousness and simplicity. The drawbacks of 60 min. Sonication with pulse duration of 5 s and a resting interval
SFE are the need for more expensive equipment and the difficulty of 5 s permitted to improve the antioxidant yield by 22% and
of extracting polar molecules without adding modifiers to CO2. reduced extraction time by 87%, and continuous UAE allowed to
Indeed, ultrasound permits the extraction of a wide variety of increase the yield by 24% and reduced the extraction time by
compounds using polar or non-polar solvents and much simpler 90%, compared to conventional maceration. In brief, the use of
equipment. When combined with supercritical fluid extraction, ultrasound enable to intensify and largely maximize the yield of
US enhance the mass transfer of the species of interest from the extraction and antioxidant activity, while decreasing energy
solid phase to the solvent used for extraction (Fig. 10 c) [82]. consumption and extraction time. Hammi et al. [89] has also
Table 2
Applications of UAE in the extraction of compounds from fruit and vegetables.
Matrix Extract Processing device Experimental conditions Reference

2
Pomegranate peel Antioxidant US probe (20 kHz, 1.267 cm ) Pulse = 5 s on, 5 s off [88]
IP = 59.2 W/cm2
T = 25 C
t = 60 min
ratio: water/peel, 50/1 (w/w)
Zyzyphus lotus fruit Antioxidant US bath (360 W) Pulse = 2 s on, 2 s off [89]
T = 63 C
t = 25 min
ratio solvent/solid: 67 mL/g
Solvent: ethanol (50%)
Tomato pomace Carotenoids (all-trans-lycopene, US probe (20 kHz, 13 mm) A = 58145 lm [90]
b-carotene) T = 25 C
t > 10 min
m = 3 g, V = 100 mL
Solvent: hexane/ethanol (50:50, v/v)
Pomegranate (Punica granatum) Natural color US probe (20 kHz) P = 80 W [91]
rinds T = 25 C
t = 30 min to 3 hours
m = 1 g, V = 50 mL
solvent: water
Jabuticaba (Myrciaria cauliflora) peel Phenol (ellagic acid), anthocyanin US bath (25 kHz, 150 W, 2.7 L) T = 30 C [93]
(cyaniding-3-O-glucoside) t = 10 min
Solvent: ethanol:water (pH = 1)
Ratio: 46% (v/v)
Garlic (Allium sativum) cloves Aroma US bath (35 kHz) T = 25 C [92]
t = 30 min
3 times extraction (V = 50 mL)
Solvent : diethyl ether, hexane, ethyl acetate
Grape (Vitis vinifera) seeds Phenol, antioxidants, US bath (40 kHz, 250 W, 10 L) T = 3367 C [94]
anthocyanins t = 1634 min
m = 2 g, V = 100 mL
Solvent: ethanol
Ethanol concentration: 3367%
demonstrated the efficacy and absence of degradation for complex mixtures of mono- and sesquiterpene hydrocarbons,
ultrasound-assisted extraction of antioxidant from Zyzyphus lotus and oxygenated materials biogenically derived from them [97].
fruit. The optimum operating conditions reported by the author Assami et al. [98] describe the use of ultrasound for aromas
was ethanol concentration of 50%, extraction time of 25 min, recovery where a US-assisted Clevenger (or sono-clevenger) is
extraction temperature of 63 C for reach a high phenolic content compared to conventional Clevenger for the extraction of aromas
of 40.78 mg gallic acid equivalent/g dry matter and DPPH activity from caraway seeds. Both extraction procedures are given here-
of 0.289 mg/mL. after: conventional extraction is performed using 150 g of seeds
The use of ultrasound has also been proved as a promising tech- finely ground to 18.0250 lm size in electric grinder for 20 s at a
nology to extract carotenoids from tomato by-product (skin, seeds, speed of 20,000 rpm using a cooling water system in order to pre-
and part of the pulp) [90]. Ultrasound significantly increased the vent volatile loss during milling. The resulting mixture is then sub-
extraction yield of 143% in comparison with conventional extrac- mitted to hydro-distillation for three hours. For US-assisted system
tion and did not cause any degradation of carotenoids. Sivakumar a 3L double jacketed reactor composed of an inox jug
et al. [91] has reported the significant improvement (13100%) of (23 cm 13.7 cm) and operating at a frequency of 25 kHz and at
the extraction yield of the natural colors obtained from different an intensity of 1 W/cm2 was used. The mixture was homogenized
plant materials. Kimbaris et al. [92] have demonstrated that the thanks to a rotating pale and US was then applied for 30 minutes.
use of ultrasound for essential oil extraction from garlic reduced For each experiment the mixture composed of 150 g of crushed
the degradation of thermal-sensitive molecules, compared to material with 1.5 L of water (same ratio as the conventional extrac-
hydro-distillation. tion) was placed into the reactor and after the US treatment the
resulting mixture was submitted to a Clevenger hydrodistillation
5.2. Herbs and spices for the recovery of the essential oil. Both extracts are qualitatively
and quantitatively analyzed by GCMS and a selectivity is noticed;
Herbs and spices are commonly used for food, cosmetic or phar- the ultrasonic treatment has a clear influence on the recovery of
maceutical applications as sources of various compounds of inter- carvone and limonene when compared to untreated seeds.
est such as antioxidants, capsaisinoids, aromas, flavors, fragrances Other compounds such as capsaicinosids (noridihydrocapsaicin,
or volatile compounds that can be extracted from different capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocap-
matrices such as pepper, rosemary or caraway seeds for example. saicin) can be extracted from pepper (Capsicum frutescens) and by
Ultrasound can successfully be applied in the recovery of aroma changing solvent in the US-assisted extraction, selectivity has been
molecules which are conventionally extracted by hydro- observed among those compounds [99,100]. The possibility of
distillation [95] from a large range of herbs and spices using a selecting the compound of interest by US-assisted extraction can
Clevenger-type system at lab scale [96]. Flavors and fragrances be observed for caraway seeds, as described before, where at low
are complex mixtures of volatile compounds which consist in temperatures, a selectivity is observed for carvone extraction
instead of limonene [39,98]. It can also be observed for US-assisted and placed in the cellulose thimble plugged with cotton and placed
extraction of rosemary where carnosic acid is better extracted from in the extraction chamber. The Soxhlet apparatus is then placed
dried material in ethanol, while rosmarinic acid is better extracted into a thermostated water-bath. The sonicator probe is placed at
using methanol as solvent [101,102]. Several applications of the 1 mm from the surface of the Soxhlet chamber with an inclination
use of UAE for different target compounds from several herbs angle of 45 with respect to the vertical position and at 9 cm height
and spices are given in Table 3, with the UAE conditions. from the bottom of the water bath. The extraction program consist
of a number of cycles that depends on the extraction kinetics of the
5.3. Oleaginous seeds target compound. Each cycle involves three steps: (1) filling of the
Soxhlet chamber by solvent evaporated from the distillation flask,
Oleaginous plant seeds are a renewable resource available condensate in the refrigerant, and dropped on the sample; (2)
worldwide. Soybean alone represents over 70% of world produc- ultrasound irradiation of the cartridge for 10 s (duty cycle 0.5 s,
tion, followed by sunflower and rapeseed representing approxi- output amplitude 40% of the nominal amplitude of the converter,
mately 15% each. In Europe the most cultivated is rapeseed far applied power 100 W); (3) unloading of the Soxhlet chamber con-
ahead sunflower, soybean and also flaxseed taking an honest share tent after the solvent extraction reach the siphon height. After the
in France. Oleaginous seeds can also be found in fruits (nuts, extraction, the content of the flask is evaporated under reduced
almonds, papaya seeds, fruits kernels) [107]. pressure. Several applications of the use of US for the extractions
Fats and oils are a main source of energy used by the body. of compounds, mostly oil, from several oleaginous seeds are given
Moreover, they participate in the transmission of nerve impulses, below, in Table 4, with the UAE conditions.
maintain the integrity of cell membranes, have a role in cellular
transport, and are precursors of many hormones. From all sources 5.4. Microorganisms
of lipid, oil seeds are complex matrices from which it is possible to
extract monoacyl glycerols (MAG), diacyl glycerols (DAG), triacyl Microorganisms such as bacteria, yeast, fungi, and microalgae
glycerols (TAG), and free fatty acids (FFA) associated with other are able to produce primary and secondary interesting metabolites
minor compounds, also called micronutrients, such as pigments, as pigments, antioxidants, polysaccharides, acids, lipids employed
sterols, antioxidants, alkaloids [108]. Oils are usually analyzed by for cosmetic, food, pharmaceutic and biofuel applications. In
GC-FID, after transmethylation of acylglycerols, in order to deter- oleaginous microorganisms, lipids are found mainly in the form
mine their fatty acid profile and investigations on minor compo- of neutral lipids, glycolipids, phospholipids, and free fatty acids
nents are generally conducted with HPLC analysis. (FFA) [115]. Some strains with optimized culture conditions are
The conventional methods for seed oil extraction are hot or cold able to content up to 70% w/w on dry biomass weight basis
pressing like for flaxseed, solvent extraction (Soxhlet), and eventu- [116], thus are recognized as a promising source of feedstock for
ally combination of processes like for rapeseed. Pressing is an old biodiesel production. Conventional methods used for lipid extrac-
technique to squeeze the oil out of solid residue [109], nevertheless tion from oleaginous microorganisms involve organic solvent
matrix containing more than 30% oil, such as rapeseed containing extraction using non-polar or low polar solvents such as chloro-
nearly 50%, require more than a simple pressing to recover the form or hexane [117].
maximum oil contained in the seed. A first prepressing is realized The most cited reference method for lipid extraction from bio-
in order to remove part of the oil from the matrix, press-cake is logical materials is Bligh and Dyer [118]. It is an economical adap-
then subjected to solvent extraction [109]. Industrially, solvent tation of the Folch procedure [119] which consists in a mixture of
extraction step is generally performed in countercurrent extractors chloroform and methanol, forming a monophasic solvent system,
using large amounts of hexane. to extract and dissolve the lipids. Adam et al. [120] have reported
Conventional Soxhlet extraction [110] is performed according a study on an innovative technique such as solvent-free
international standard NF EN ISO 659 [111]. Ultrasound has suc- ultrasound-assisted extraction for lipid recovery from fresh Nan-
cessfully been applied to the Soxhlet extraction using a sono- nochloropsis oculata microalgae biomass in comparison with the
soxhlet [76,77]. As for conventional Soxhlet, the sample is weighed conventional extraction methods. The conventional procedure for
Table 3
Applications of UAE in the extraction of compounds from herbs and spices.
Matrix Extract Processing Experimental conditions Reference

device
Rosemary Antioxidants (carnosic acid, ursolic acid) US bath S/L ratio = 1/20 (m/V), Solvent = EtOH/H2O, 90/10 (V/V), [103]
US reactor t = 30 min, T = 40 C
(150 W)
US probe
(1 kW)
Pepper Capsaisinoids US bath m = 0.22 g, V = 1550 mL, solvent = MeOH, EtOH, acetonitrile, [99]
(360 W) MeOH/H2O (0100%), t = 225 min, T = 1060 C
Caraway seeds Carvone, limonene US reactor I = 1 W/cm2, m = 150 g, V = 1.5 L, solvent = water, t = 30 min, [98]
(25 kHz) Hydrodistillation
Marjoram Antioxidants (rosmarinic acid, carnosic acid, US probe m = 0.5 g, V = 25 mL, solvent = MeOH/H2O 80/20 (V/V), t = 5 [104]
luteolin-7-O-glucoside, apigenin-7-O-glucoside) (20 kHz, 15 min, T = 1535 C, pulse = 5 s on, 5 s off
19 mm)
Saffron Volatile compounds US bath M = 50 mg, V = 1 mL, solvent = MeOH/acetonitrile 38/62, (V/V), [105]
t = 22 min
Spearmint Flavor volatile compounds US probe Amplitude = 25%, m = 50 g, V = 100 mL, solvent = EtOH/H2O 70/ [97]
(Mentha (200 W) 30, (V/V), t = 5,10,15 min, T < 40 C
spicata)
Tea Aroma compounds US bath m = 3 g, V = 300 mL, solvent = water, t = 40 min, T = 60 C [106]
(40 kHz,
250 W)
Table 4
Applications of UAE in the extraction of compounds from oleaginous seeds.

Soybean, Oil US probe/Soxhlet m = 10 g, V = 100 mL, solvent = hexane, Irradiation time = 10 s (after the solvent [76]
sunflower, rape reach the siphon height)
Almond Oil US bath (40 kHz, 150 W) Solvent/sample ratio = 1020(mg/L), solvent = hexane, t = 4060 min, T = 40 [75]
60 C
Papaya seed Oil, US bath (40 kHz, 700 W) P = 235700 W, Sample/liquid ratio = 6/110/1 (V/w), solvent = hexane, t = 5 [112,113]
antioxidants 30 min, T = 2550 C,
Pistacia khinjuk Oil US probe (30 kHz, 100 W, Amplitude = 0, 25, 50%, pulse = 10 s on, 5 s off, ratio = 1/4 (w/V), [114]
kernel diameter = 10 mm) solvent = hexane, T = 30, 40, 50 C
Flaxseed Oil US probe (20 kHz, 250 W) P = 50 W, ratio = 6/1 (V/w), solvent = hexane, V = 100 mL, t = 30 min, T = 30 C [73]
Soybean Oil US bath I = 47.6 W/cm2, solvent = hexane/isopropanol (3/2) [63]
lipid extraction from microorganisms is a Bligh and Dyer modified methanol) gave higher yields for carotenoids and chlorophylls as
procedure. A solution of EDTA (1 ml, 1 mM in 0.5 M acid acetic) well as for carotenoids/chlorophylls ratio. Another study based
was mixed to 10 mg of wet microalgae (20% dry weight). The mix- on a comparative study of carotenoids and fatty acids extracted
ture was transferred to a glass tube with 3 mL of chloroform: from Synechococcus sp. with supercritical fluid and UAE using
methanol (1:2, v/v), then covered with a screw cap in Teflon and DMF. UAE allows higher concentrations of b-carotene than
vortexed (VX-2500, VWR). After, 1 mL of chloroform and 0.8 mL supercritical fluid, although the recovery of astaxanthin with ultra-
of KCl (0.88%, w/v) were added before being vortexed and cen- sound is low compared to SFE [125]. Table 5 presents applications
trifuged at 4000 rpm for 2 min. The lower chloroform phase was of UAE for obtention of high value compounds from various
pipped and placed to a new glass tube. Cells were then extracted microorganisms.
again with hexane, centrifuged and the supernatant was combined
with the previous chloroform extracts. Finally lipid extracts were 6. HACCP and HAZOP considerations using UAE
dried under a stream of N2 and re-suspended in solvent for further
analyses by GCFID analysis. Ultrasound-assisted extraction was HACCP (Hazard Analysis and Critical Control Points) concept is a
performed with success using a standard titanium sonotrode (area systematic approach to food safety management based on 7 recog-
of 9 cm2) combined to a booster and operating at 20 kHz with a nized principles designed to identify and prevent the hazards likely
1000 W ultrasonic processor. For each experiment 100 g of wet to occur at any stage in the food supply chain [128]. A critical con-
N. oculata (30% dry weight) was submitted to sonication. An exper- trol point (CCP) is a step in the flow diagram of the food process at
imental design through response surface methodology (RSM) which control measures can be applied. These CCPs are essential to
parameters was used and optimum conditions for oil extraction prevent or eliminate a food safety hazard or reduce it to an accept-
were estimated as follows: 1000 W ultrasonic power, 30 min able level.
extraction time and biomass dry weight content at 5 %. This study Ultrasound is nowadays commonly used in many unit opera-
on non-starved microalgae has proved the efficiency of ultrasound tions during food processing considering their physical effects for
for oil recovery in a reduced time and with a simple and scalable extraction, degassing or cutting, but also considering their chemi-
pre-industrial device. These conclusions were also supported by cal and biological effects for the inactivation of enzymes or the
Piasecka et al. [121] for lipid extraction from Chlorella protothe- sterilization of equipment for example. However, the use of US in
coides microalgae. The ultrasonic pretreatment has improved the food engineering requires the setting-up of an HACCP program in
extraction yield of 42% and the palmitic acid content in the fatty which the CCPs are identified, so that potential hazards in produc-
acids profile. Other microorganisms such as oleaginous yeast ing a safe quality product can be controlled. These can be biologi-
Trichosporon oleaginosisus (ATCC20509) and oleaginous fungus cal, chemical or physical hazards that need verification activities.
(SkF-5) was also extracted by ultrasound in order to promote the Examples are given in Table 6. In the ultrasound treatment, the
lipid recovery [122]. In this case, ultrasonication of oleaginous critical processing factors are assumed to be the amplitude of the
microorganisms mixed with conventional solvent mixture (chloro- ultrasonic wave, the time of exposure/contact with the microor-
form:methanol) allows to reduce extraction time from 12 hours to ganisms, the type of microorganism, the volume of food to be pro-
15 min in comparison with the conventional method, without cessed, the composition of the food, and the temperature of the
affecting fatty acids profile of the biofuel. treatment. During the development of the HACCP plan, the HACCP
Ultrasound-assisted green solvent extraction is also a promising team must establish procedures to be followed if and when the
tool for recovering of other high-value compounds such as pheno- monitoring of a CCP reveals that the critical limits are not
lic compounds and chlorophylls from microorganisms such as respected, and therefore there is a loss of control of the hazard at
Nannochloropsis spp. microalgae [123]. The extraction yield of the CCP. A product that is obtained during a processing step where
these high-value compounds was two times higher by UAE in the CCPs are not respected is described as non-conform and is
comparison with conventional water extraction by maceration. likely to be unsafe if consumed.
Optimum operating conditions in order to obtain the maximum Hazard and operability (HAZOP) study is a formal, systematic,
yield was 400 W, 5 min of sonication, and a binary mixture of logical, structured investigative study for examining potential
solvents such as water:DMSO and water:EtOH. deviations of operations from design conditions that could create
Natural colors are very demanded by food and cosmetic indus- processoperating problems and hazards [129]. It is one of the
tries as additives. Macias-Sanchez et al. [124] have proposed a most structured techniques to identify hazards in a process plant
comparative study of two innovative techniques: UAE and super- and aims to find all possible deviations from the normal function-
critical fluid for extraction of carotenoids and chlorophyll from ing of process parameters. HAZOP study analysis is the key critical
Dunaliella salina. The study indicates that the supercritical fluid tool used throughout processing industries worldwide. The tech-
extraction process is comparable to the ultrasound-assisted extrac- nique was designed to optimize the process and improve perfor-
tion when methanol is used as solvent. In the case of UAE, the sol- mance. The purpose of the study is to provide a list of issues and
vent N, N-dimethylformamide, DMF (more selective than recommendations for the prevention of each problem [129].
Table 5
Applications of UAE in the extraction of compounds from microorganisms.

Nannochloropsis oculata microalgae Lipids US probe t = 30 min [120]
(20 kHz, 1000 W, biomass dry weight 5%
9 cm2) solvent free
Trichosporon oleaginosisus yeast and Lipids US horn (520 kHz, T = 25 C [122]
oleaginous fungus (SkF-5) 40 W) t = 15 min
US bath (50 Hz, Solvent: chloroform/methanol (1:2, v/v)
2800 W)
Nannochloropsis spp microalgae Phenolic compounds and US probe (24 kHz) P = 100400 W [123]
chlorophylls T < 60 C
t < 30 min
m = 250 g suspended in Ethanol and DMSO
Dunaliella salina microalgae Carotenoids and chlorophyll US bath t = 3 min [124,125]
Synechococcus sp. cyanobacteria m = 0.105 g of lyophilized microalgae in 5 mL
DMF and methanol
Xanthophyllomyces dendrorhous yeast Carotenoids (astaxanthin) US bath T = 4060 C [126]
t = 1535 min
0.2 g lyophilized biomass in 10 mL of 5 mol/L
lactic acid.
Cordycepssinensis fungus Water-soluble components and US probe (20 kHz) UI = 2.4444.1 W/cm2 [127]
polysaccharides T = 4070 C,
particle size = 156.5750 lm solid/liquid
ratio = 1/301/70 g/mL
Table 6 and 0.25 kW.h for UAE (electrical energy for ultrasound supply).
Examples of verification activities for CCPs. The power consumption was determined with a Wattmeter at
the ultrasound generator supply and the electrical heater power
Danger types Verification activities
supply. Regarding environmental impact, the calculated quantity
CCPs for Biological Hazards
of carbon dioxide rejected in the atmosphere is higher in the case
Sterilization Review of pasteurization, records, microbiological testing
of product periodically of Soxhlet (6400 g CO2/100 g of extracted solid material) and mac-
Acidification Review of pH measurement records, microbiological eration (3600 g CO2/100 g of extracted solid material) than for UAE
testing of product periodically (200 g CO2/100 g of extracted solid material). These calculations
CCPs for Chemical Hazards have been carried out based on the following assumptions: to
Receiving of raw Review of certificates of analysis, periodic sampling and obtain 1 kW.h from coal or fuel, 800 g of CO2 will be rejected in
material testing of raw material
the atmosphere during combustion of fossil fuel. UAE is thus pro-
Labeling Review of labeling inspection records
posed as an environmentally friendly extraction method suitable
CCPs for Physical Hazards
for extraction at laboratory scale but could be also transposed to
Filtering Review of filter inspection records
Metal detection Review of metal detector records
pilot and industrial scale.
The main hazard the users may face is from accidental contact 8. Up-scaling of UAE and its applications in industry
exposure to the ultrasonic waves. Direct contact exposure can
cause tissue injury for the operator. Moreover, ultrasound equip- To ensure safety, sustainability, economic and greener methods,
ment are electrical devices that may present danger to operators. the design of an efficient ultrasound-assisted large-scale extraction
Electricity can cause electrical shock and burns, and be a potential requires process intensification and energy consumption reduc-
fire hazard. Ultrasound can also generate indirect effects on the tion. Both types of devices for high power ultrasound such as probe
operator: (i) airborne ultrasound: it can affect the central nervous and bath systems are widely used industrially, due to their differ-
system and imply damages to the ear, (ii) heat and cavitation: it ence of potential and efficiency, the choice of the system will
can cause burns and chronic lengthy exposures could raise body depend of the matrix and the application desired. Hielscher
temperatures to mild fever levels during the exposure periods. (Germany) and REUS (France) are the main companies which
develop large-scale ultrasound extraction devices. The major
7. Environmental impact of Ultrasound-assisted extraction parameter for an industrial setup is the quantity of product to be
(UAE) treated, ultrasonic probe are restricted for the small volume. One
solution is the use of a continuous system that can handle a larger
UAE is a clean method that avoids the use of large quantity of amount with a restrictive volume of reactor, ultrasound are then
solvent and voluminous extraction vessels like Soxhlet and macer- more concentrated with a maximum power per volume. Hielscher
ation. The reduced environmental impact of UAE is clearly advan- Company commercializes devices of a wide range power from 50
tageous in terms of energy and time. As an example, extraction of to 400 W for analytical scales and from 500 to 16,000 W in indus-
fat and oil from oleaginous seeds is performed with Soxhlet proce- trial scales (Fig. 11). The other alternative is to use ultrasonic baths
dure, which needs to extract 50 g of seeds with 300 mL of hexane with a larger radiating surface and an agitation system. REUS Com-
as solvent for 8 hours. The energy required to perform the three pany has developed a wide range of reactors from pilot (30 to 50 L),
extraction methods are respectively 6 kW.h for maceration at the and industrial scale (500 to 1000 L), coupled with pump systems in
solvents boiling point (electrical energy for mechanical mixing order to fill the ultrasonic bath, to stir the mixture and to empty
and for heating), 8 kW.h for Soxhlet (electrical energy for heating), the system at the end of the procedure (Fig. 12).
Fig. 11. Industrial ultrasonic continuous equipments (Hielscher www.hielscher.com).
Fig. 12. Industrial ultrasonic batch equipments: 50, 500 and 1000 L (Reus www.etsreus.com).
An increasing number of companies already use the ultrasonic an Italian company specialized in natural extracts from herbs,
technology, either by adapting their conventional or innovative fruits and vegetables using ultrasound technology to improve the
system of extraction or by changing their installation. In industrial flavor and quality of the extracts. GMC (G. Mariani & C. Spa) com-
scale, the majority of extracted compounds is directly used, as in pany has also adapted their conventional extraction system in
liquor production or can be used as food and cosmetic additives, order to intensify aromatic herbs extracts. Giotti (Italian company)
in the case of essential oil and bioactive molecules. Euphytos is is equipped by four continuous batch systems coupled with
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Ultrasound assisted extraction of food and natural products.

4. Ultrasound techniques for extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548

1. Introduction Ultrasound is a key-technology in achieving the objective of

Fig. 1. Ultrasound-assisted extraction: evolution or revolution.

2.1. Fragmentation 2.2. Erosion

Matrix Extract Processing device Experimental conditions Reference

Matrix Extract Processing Experimental conditions Reference

Matrix Extract Processing device Experimental conditions Reference

Matrix Extract Processing device Experimental conditions Reference

Fig. 11. Industrial ultrasonic continuous equipments (Hielscher www.hielscher.com).

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