Journal of Drug Delivery Science and Technology 75 (2022) 103687

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Journal of Drug Delivery Science and Technology

journal homepage: www.elsevier.com/locate/jddst

Short communication

Scope of solid lipid nanoparticles per se as all-purpose

moisturising sunscreens
Garima Sharma a, 1, Garima Khanna a, 1, Shivam Gupta a, Mohhammad Ramzan a, b, Joga Singh a,
Mandeep Singh a, Ujjesha Mudgill a, Jaspreet Singh Gulati c, Indu Pal Kaur a, *
a
University Institute of Pharmaceutical Sciences, Panjab University, Chandiagrh, 160014, India
b
School of Pharmaceutical Sciences, Lovely Professional University, Punjab, 144402, India
c
Hitech Formulations Pvt Ltd, Chandigarh, 160002, India

A R T I C L E I N F O A B S T R A C T

Keywords: Sun blocking effect is defined as the ability to protect the skin against ultraviolet-induced damage, indicated in
Photoprotection terms of sun protection factor (SPF). This protection can be physical or chemical. Chemical sun protecting agents
Skin cancer can permeate the skin leading to toxic side effects. Solid lipid nanoparticles (SLNs), also known as lipid carriers
Dermatology
have been widely investigated across the world and have evolved as promising nano-sized drug carriers. In this
Cosmetic
Skin hydration
study, different placebo SLN formulations demonstrate sun protection. Five different SLN formulations (F1–F5)
Photoageing with varying lipid content were developed using three industry amenable techniques viz. high speed stirring
(HSH), high pressure homogenisation (HPH) and microemulsification method (MEM). A correlation between
morphology (HR TEM), particle size-polydispersity index (DLS), sun protection factor (SPF) and occlusive effect
(OE) were established. Results indicated promising SPF (6.0–24.0) and hydrating effects (OE 6.0–71.0) of
spherical, mono disperse lipidic nanoparticles with lipid content of ≥4%. SLNs were found to offer hydration
effects comparable to Vaseline® petroleum jelly (OE 71.0 and 82.0, respectively). Hence, SLNs per se can be
regarded as: (i) safe alternative to current toxic chemical sunscreen agents, or (ii) carriers for latter, employed at
low concentration to provide similar effects, and (iii) as suitable moisturisers.

1. Introduction UV radiation [2].

However, there is growing public concern about the negative con­
Sunshine is beneficial to our skin because it supplies essential vita­ sequences of chemical sunscreens viz. erythema, edema, and irritation.
mins to our body and promotes the production of hormones such as The three primary groups of compounds that are especially worrying
serotonin. However, excessive UV exposure can damage DNA, connec­ include benzophenones, camphor derivatives, and cinnamate de­
tive tissue or collagen, causing avariety of health issues, including hy­ rivatives. Benzophenone was once commonly used in sunscreen prepa­
perpigmentation, loss of elasticity, burns, ageing photoaging and rations, however its remains have been detected in waste water, human
increased risk of developing skin cancers [1]. Due to such detrimental urine and breast milk [3]. Camphor derivatives are utilised as UVB ab­
effects of sun rays, the usage of sunscreen preparations is recommended. sorbers and aggregate in tissues after extended exposure, and because
Sunscreen efficacy is defined as the capacity to safeguard the skin from they are extremely lipophilic, they can be quickly absorbed after direct
ultraviolet-induced burning, with the level of performance represented skin contact [4]. Cinnamate derivatives are known to cause photosen­
by the sun protection factor (SPF). Primary and secondary protective sitivity, allergic contact dermatitis and photocontact dermatitis. Octyl
factors are involved in photoprotection. Sunscreens are primary con­ methoxycinnamate, which is a potent UVB blocker, is reported to pro­
tributors; and include physical barriers that reflect and scatter light as duce harmful free radicals upon its absorption through skin [5,6]. Since
well as chemical barriers which absorb light. Secondary factors such as sunscreen application is not dose-controlled, hence it is difficult to
antioxidants, osmolytes, and DNA repair enzymes assist to minimize research their toxicity, and most observations are based on animal
skin damage by interfering with the photochemical cascade caused by studies. Customer safety concerns about sunscreens cannot be dismissed

* Corresponding author. University Institute of Pharmaceutical Sciences, Panjab University, Chandiagrh, 160014, India.
E-mail address: [email protected] (I.P. Kaur).
1
Both the authors contributed equally to the work.

https://doi.org/10.1016/j.jddst.2022.103687
Received 26 March 2022; Received in revised form 15 July 2022; Accepted 6 August 2022
Available online 12 August 2022
1773-2247/© 2022 Elsevier B.V. All rights reserved.
G. Sharma et al. Journal of Drug Delivery Science and Technology 75 (2022) 103687

without more investigation, and further research is required [7]. Phys­ transepidermal water loss (TEWL) achieved by formation of an imper­
ical sunscreen ingredients on the other hand though safe, are opaque and meable barrier of collapsed lipidic nanoparticles on skin [16]. This
cause the skin to look white following application. The advancement of barrier formation is attributed to intrinsic particulate nature, film
nanotechnology [8] and the creation of nanosized zinc oxide and tita­ forming and lipo-occlusive property of SLNs. The extent of occlusive
nium dioxide has enabled formulators to make more effective and effect also depends on the particle size and lipid content [17]. The
cosmetically appealing sunscreen creams, without producing local adhesiveness of a material is associated with its fineness, lower the
adverse effects other than the formation of free radicals, that may be particle size better the adhesive properties [18]. Earlier in 1998, ac­
carcinogenic [9]. In order to improve sun protection efficacy, manu­ cording to Muller-Dingler the monolayer of spherical particles were
factures must overcome current crucial obstacles such as the growing assumed to form a hexagonal packaging having free/uncovered area in
prevalence of melanoma risk, eczema, or photo allergies caused by between, called as voids or holes. These holes are large for bigger par­
sensitization interactions between chemical sunscreens and the skin. ticles which are responsible for evaporation of water from the skin.
Solid lipid nanoparticles (SLNs) are colloidal carriers that have been Whereas in smaller particles (nano) the void volume is very less
designed as a replacement for conventional carriers. Considering their which unlike microparticles favors water condensation leading to in­
particulate nature, uniform size, smaller surface area, and excellent crease in vapor pressure and hence reduced TEWL [19]. The theory was
drug-loading capacity, SLNs are becoming increasingly popular [1] and later updated by Muller et al., as per this theory the loss of water from
have been proven to serve as active carriers for sunscreens. The encap­ SLNs forms a compact impermeable layer responsible for reduced water
sulation of molecular sunscreens in SLNs has a synergistic effect on its loss from skin and improved moisturisation [20]. Further, the increased
protective properties. Because SLNs function as physical sunscreens on skin hydration levels also provide anti-damage effects like better elas­
their own, the concentration of potentially harmful molecular sunscreen ticity to the skin. Dryness and loss of elasticity is usually observed with
can be reduced while retaining the sun protection effect. SLNs, the sun exposure/photoageing and is responsible for wrinkle formation
prolonged release carrier system for the encapsulated active, can ensure [21].
that the sunscreen remains on the skin’s surface for longer times [10]. Presently, we designed, developed and evaluated different lipids at
Highly crystalline SLNs can act as particulate UV blockers which work varying concentrations for preparing SLNs. The placebo SLNs formu­
by scattering the light efficiently (Fig. 1). They show various advantages lated using different preparation methods were analysed for sunscreen
such as feasibility of incorporation of lipophilic and hydrophilic sun­ and occlusive effects which was correlated to their composition and
screen actives, improved physical stability, low cost compared to lipo­ particle size. Sunblocks reflect UV rays and provide photoprotection
somes and ease of scale-up and manufacturing. Moreover, controlled while, sunscreens absorb UV rays. SLNs partly reflect and partly absorb
release of the sunscreen from the SLNs can reduce dose limited side UV rays owing to their particulate nature, which suggests their dual
effects. Further suitable size modulation can control permeation of these implication as sun protection agents.
particles beyond epidermis. Latter is achieved by size regulation and
composition which restricts permeation of SLNs beyond epi/­ 2. Materials
hypodermis, if required for topical delivery [11,12].
SLNs are reported to be safe for dermal application and are even Compritol® 888 ATO was received from Gattefosse, France, as gift
compatible for use on inflamed skin due to the non-skin irritation and samples. All the other related material including lipid A and B were
non-toxic properties of the lipid matrix [13]. Several different type of obtained from Hitech Formulations Private Limited, Chandigarh as
SLN formulations from our lab have also been tested to be safe for gratis.
dermal use, both in vitro (cytotoxicity studies) and in vivo as per OECD
guidelines [12–15].
3. Methods
Further SLNs not only act as physical sunscreens but also manifest
moisturising effects. They possess a unique potential to collapse and
3.1. Preparation of solid lipid nanoparticles (SLNs)
form a continuous occlusive film on the skin surface following evapo­
ration of water present in the formulation (Fig. 1). The formed occlusive
Five different formulations (Table 1) with lipid content ranging from
film, which shows high affinity towards stratum corneum tends to
4% to 16% were prepared using three different methods viz. high speed
maintain good skin hydration levels. Latter is due to reduction in
stirring, high pressure homogenisation and microemulsification method

Fig. 1. Diagrammatic representation of sun protection and occlusive property of SLNs.

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G. Sharma et al. Journal of Drug Delivery Science and Technology 75 (2022) 103687

Table 1
Description of different SLN formulations (F1–F5) along with particle size (PS) and polydispersity index (PDI).
Formulation Lipid Total lipid content Particle size PDI Method

F1 Compritol® 888 ATO 4% 320 ± 40 nm 0.17 High Pressure Homogenisation

F2 Compritol® 888 ATO 5% 130 ± 25 nm 0.11 Microemulsification
F3 Compritol® 888 ATO + Lipid A 9% 285 ± 65 nm 0.27 Microemulsification
F4 Compritol® 888 ATO 10% 292 ± 47 nm 0.14 High Pressure Homogenisation
F5 Compritol® 888 ATO + Lipid B 16% 235 ± 50 nm 0.18 High Speed Stirring

as described below. and Abs is absorption of test sample at wavelength (λ).

High speed stirring (HSS): Lipid phase containing either a combination
of high melting point lipids or lipid-oil and/or surfactant was heated at
5 ◦ C above their melting points. An aqueous phase containing water and 3.5. In-vitro occlusivity test
surfactant (previously maintained at the same temperature as lipid
phase) was added to the lipid phase under continuous stirring at The occlusive effect of different SLN formulations was determined
500–800 rpm for 45–60 min to result in a coarse pre-emulsion. This pre using previously described method [17], with few modifications. Glass
emulsion after cooling at room temperature was subjected to high speed beakers of equal dimension (6.28 cm2) were employed in the study to
stirring at 10,000–12,000 rpm for 15 min to result in solid lipid nano­ minimize any errors due to change in exposed surface area. All the glass
particles (F5). beakers (n = 3) were filled with 10 mLwater. The mouth of the beaker
High pressure homogenisation (HPH): After formation of primary was covered completely with Whatman® filter paper and the edges were
emulsion as stated above in HSS method, the coarse emulsion was sealed properly with para film/tape to avoid any loss of water along the
passed through a HPH for 3–7 cycles to result in SLNs after cooling at sides. An equal amount (100 mg) of various test formulations including
room temperature (F1 and F4). Vaseline® (standard reference) was spread evenly on the Whatman®
Microemulsification method (MEM): Unlike above two methods where filter paper to form a thin film. The glass beaker with Whatman® paper
pre emulsion was white and coarse in nature, the emulsion in this case but no formulation served as blank. Prior to the placement of beaker in
was a clear microemulsion. Latter was poured into an equal quantity of incubator shaker (32 ◦ C, 100 rpm), each beaker assembly was weighed
cold water (0–4 ◦ C) under continuous stirring with a mechanical stirrer to note the initial weight. The beakers were carefully withdrawn from
at 2000–3000 rpm for 45–60 min to result in SLNs (F2 and F3). the incubator and weighed at different time intervals of 6,12, 24 and 72
All the SLN formulations described above were pre-optimized for h to measure the loss of water from the beaker. The occlusivity (F) of
desired particle size and stability. Concentration and type of lipid was each formulation was deduced using equation:
decided to achieve desired particle size (<500 nm and PDI <0.3)
Water ​ loss ​ without ​ sample − water ​ loss ​ with ​ sample
employing safe and minimal surfactant concentrations. F= × 100
Water ​ loss ​ without ​ sample

3.2. High resolution transmission electron microscopy (HR TEM)

4. Results

The developed SLNs were suitably diluted before their morpholog­

4.1. Preparation of SLNs
ical evaluation using high resolution transmission electron microscopy
(HR-TEM, H-7500 Hitachi). A drop of aqueous dispersion of each
All the five formulations (F1–F5) were prepared using high melting
formulation (F1–F5) was placed on a carbon coated copper grid and air
point lipid Compritol® 888 ATO which is a mixture of mono-, di- and tri-
dried before analysing under HRTEM.
esters of behenic acid, with diester being the predominant fraction.
Some formulations included other lipid components viz. Lipid A (F3)
3.3. Particle size and polydispersity index (PDI) and Lipid B (F5) (Table 1). The total lipid concentration in the formu­
lations F1 to F5 varied from 4 to 16% to result in different consistency
The particle size and PDI analysis of all the SLN formulations (F1–F5) and nanoparticulate nature. Apart from lipids, all the formulations
were done using Delsa™ Nano C, Beckman Coulter, USA, after their contained a similar surfactant and co-surfactant ranging from 12 to 30%
suitable dilution with Milli-Q water to form an aqueous dispersion of and 6–9%, respectively. The composition of formulation F1, F2 and F4
appropriate intensity. are similar except the difference in lipid content (4%, 5% and 10%),
surfactant (12% (F1, F4) and 28% (F2)) and method of preparation
3.4. Sun protection factor (SPF) evaluation (HPH (F1, F4) and MEM (F2)). The SLN formulation F1&F4 and F2&F3
were prepared using HPH and MEM, respectively (Table 1). The
Weighed amount of SLN formulations (100 mg) were dispersed in 10 composition and method of preparation for F5 varied from all other
mL of water using a volumetric flask (solution-A). Two mL aliquot of formulations.
solution-A was further diluted with water up to 10 mL (solution-B). As
done previously, a 1 mL of solution-B was further diluted with 10 mL of
water to result in ‘solution-C’. Latter was transferred into cuvettes and 4.2. HR TEM evaluation
exposed to UVB light ranging between 290 nm and 320 nm. The
absorbance was noted at an interval of 5 nm (n = 3). The obtained All SLN formulations contained spherical particles as depicted by HR
absorbance values were processed using Mansur equation [22] to get TEM images shown in Fig. 2.
respective SPF values of SLN formulations (F1–F5).
∑ 4.3. Particle size (PS) and PDI
320
SPF = C × EE(λ) × I(λ) × Abs(λ)
290
The particle size of different formulations was in the range from 100
where, values of EE (erythemogenic effect) and I (intensity of light) at nm to 350 nm, as stated in Table 1. PDI values below 0.3 indicated
particular wavelength (λ), are constant [23,24], C is correction faction, formation of uniformly distributed mono disperse systems.

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G. Sharma et al. Journal of Drug Delivery Science and Technology 75 (2022) 103687

Fig. 2. HR TEM images of SLN formulation F1–F5.

4.4. SPF evaluation (PDI) along with high lipid content plays a crucial role in blocking
harmful sun rays. While the nature of lipid and preparation method does
The SPF values (n = 3) were found to increase with an increase in not play any vital role in sun block effects.
lipid content as shown in Figs. 3–4 and Table 2. It is clear from Figs. 3
and 4 that the increase in sun block effect is directly proportional to the
4.5. In-vitro occlusivity test
lipid content. As the concentration of lipid in F1 is increased by 1.25,
2.25, 2.5 and 4 times to result in formulations F2, F3, F4 and F5, the SPF
Like what was observed in case of SPF, the occlusivity factor for each
values were also found to be affected in almost similar order as 1.63,
formulation (n = 3) was also found to increase proportionally
2.19, 3.66 and 3.50, respectively from F1–F5. The effect of particle size
(6.9–70.82) with an increase in lipid content (4–16%) with few excep­
and PDI on sun blocking efficiency is also plotted in Figs. 3 and 4,
tions (F5) (Figs. 5–7). Highest occlusive effect was achieved in formu­
respectively. It is observed that a change in particle size from 100 to 350
lation F5 (70.82) which was found to be very close to the standard value
nm does impact SPF of SLN formulations. However, uniformity in size
of 82.07 observed for F6-Vaseline® (Fig. 5). Despite of a minimal

Fig. 3. Effect of lipid content and PDI on SPF values of SLN formulations (F1–F5)
All the values are significantly different (p < 0.05) from each other except those marked similarly as *.

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G. Sharma et al. Journal of Drug Delivery Science and Technology 75 (2022) 103687

Fig. 4. Effect of lipid content and particle size on SPF values of formulations (F1–F5)
All the values are significantly different (p < 0.05) from each other except those marked similarly as *.

other adverse implications to healthy skin. Solid lipid nanoparticles due

Table 2
to their structure, size and composition are popular to overcome several
SPF values and occlusive factor for SLN formulations (F1–F5).
active pharmaceutical ingredient related issues viz. efficacy (solubility,
Formulation SPF Occlusivity permeation, controlled release), stability, and safety. Apart from these,
F1 6.2 ± 0.65 6.90 SLNs per se are also proposed to provide sun protection and occulsivity
F2 10.15 ± 1.19 62.00 (moisturising) effects [20,25,26]. Exposure to harmful UV radiations
F3 13.61 ± 1.92 37.27 often result in dry and damaged skin. An effective sunblock and mois­
F4 22.7 ± 1.28 37.81
F5 21.57 ± 1.82 70.82
turisation can be a primary protective and repair mechanism. As dis­
cussed earlier, the alleged hydration and UV protecting effects of SLNs
are attributed to the occlusive film forming potential and highly ordered
nanostructure of SLNs. The impact of lipid concentration, particle size
and symmetry on the aforementioned effects is assessed presently. SLNs
were produced using industrially reproducible methods to achieve a
desired variation in particle size and uniformity.
The SLNs were found to be spherical in shape as indicated by HR
TEM images (Fig. 2). The smallest achievable size was around 130 nm
with PDI 0.113, latter signifying high uniformity in the size. As the
concentration of the lipid was increased an increase in particle size was
observed (F2 and F3) when SLNs were produced using ME method.
However, in case of HPH the concentration of lipid was not found to be
responsible for particle size (F1 and F4) (Table 1). The SPF values were
impacted proportionally by lipid concentration. SPF of around 21–23
could be achieved with an increase in lipid content (10–16%, F4 and F5).
This can be attributed to higher crystallanity of SLNs of high lipidic
content. An exceptionally high SPF value in case of formulation F4 is
Fig. 5. Comparison of occlusivity of different SLN formulations (F1–F5) in attributed to uniform nano size (PDI 0.14) in addition to lipid content.
reference to standard F6 (Vaseline®) Further, it is also observed that the size of the particles does impact the
All the values are significantly different (p < 0.05) from each other except those sun protecting effect of SLNs as the largest nanoparticles formulation F1
marked similarly as *. with particles ranging up to 320 nm had lowest SPF value of around 6
(Fig. 4).
increase in lipid content from 4% to 5% in case of F2, a drastic increase The occlusive/moisturising effect of SLNs (F1-5) was comparable to
in occlusion (moisturising effect) was achieved due to small particle size the reference F6-Vaseline® (Table 1, Fig. 5). An improvement in
(130 nm) and its uniformity (PDI 0.11); Figs. 6–7. Similarly, formulation occlusivness was attained on increase in lipid content of SLNs. The
F3 and F4 showed comparable occlusivity (37.27 and 37.81) due to highest occlusive effect of 70.82 was accomplished in F5 (lipid 16%) and
almost identical particle size and lipid content. It may be noted that F3 lowest (6.9) in F1 (lipid 4%). F3 and F4 could achieve similar occlusivity
and F4 are completely in array when it comes to the nature of lipid used due to comparable lipid content of 9% and 10%, respectively (Figs. 5
and preparation techniques employed (Table 1). A slight increase in and 6). Both the preparations have similar particle size and differ based
occlusion/moisturising effect can also be attributed to uniform film on nature of lipid and preparation method indicating independency of
formation in case of F4 due to low PDI (Fig. 7). occlusive effect on latter. As mentioned earlier the occlusive effect of
SLNs is attributed to its ability to form a thin film resulting from evap­
5. Discussion oration of aqueous phase. Furthermore, the exceptionally high occlusive
effect shown by F2 (62.00) can be attributed to its small sized particles
An effective sun block can protect against acute and chronic ranging from 100 nm to 150 nm. Small particles demonstratelarger
impairment of skin caused by harmful UV radiations. Former is tradi­ surface area, small void volume (capillary pores) and high compaction
tionally achieved using various chemical and physical agents imposing

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G. Sharma et al. Journal of Drug Delivery Science and Technology 75 (2022) 103687

Fig. 6. Effect of lipid content and particle size on occlusivity of formulations F1–F5
All the values are significantly different (p < 0.05) from each other except those marked similarly as *.

Fig. 7. Effect of lipid content and PDI on occlusivity of formulations (F1–F5)

All the values are significantly different (p < 0.05) from each other except those marked similarly as *.

hence are highly adhesive in nature [20]. It is also known that the two Author statement
SLN formulations having equal lipid content (F1 and F2) but different
particle size have different occlusive effect, as small sized particles Indu Pal Kaur: Conceptualization, Garima Sharma, Garima Khanna,
produce higher number of particulate matter per unit area, hence denser Joga Singh, Mohhammad Ramzan, and Mandeep Singh: Methodology
film formation [17,27]. Furthermore, the uniformity in size produces and Investigation, Garima Sharma, Garima Khanna, and Shivam, Gupta:
more symmetrical films affecting the density and void volume leading to Software, Garima Sharma, Garima Khanna, Shivam Gupta and Ujjesha
high occlusive effect. As observed in Fig. 7, hydration effect was noticed Mudgill: Data curation, Indu Pal Kaur, Garima Sharma and Garima
to improve with lower PDI values i.e. more uniformity. Khanna: Writing- Original draft preparation, Indu Pal Kaur and Jaspreet
Singh Gulati: Supervision, Indu Pal Kaur: Writing- Reviewing and
6. Conclusions Editing.

Popularity of solid lipid nanoparticles as suitable drug delivery car­ Declaration of competing interest
rier has already been known for past few decades. However their use as
moisturisers and sunscreen filters per se is scarcely investigated. With an The authors declare no conflict of interest.
increase in consumer awareness towards less chemical methods and
more natural alternatives for an effective sub block, SLNs provide a wide
scope as effective moisturising sunscreens.

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G. Sharma et al. Journal of Drug Delivery Science and Technology 75 (2022) 103687

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