2nd International Conference on Oil, Gas and Petrochemical Issues(ICOGPI'2013) August 25-26, 2013 Kuala Lumpur (Malaysia)

Encapsulation ZnO Nanoparticles by

using Beeswax
Roya Namdariyan1, Afshin Farahbakhsh2* and Hossain Alizade Golestani3

Abstract— In the paper, methods for encapsulation of ZnO Bee wax is yellow, soft, biodegradable and a
nanoparticles are studied by using natural and biodegradable material considerable absorbent. It is solid at room
such as beeswax. Encapsulation is carried out for increasing temperature and insoluble in acids, alcohols and
persistence time and controlled release of nanoparticles in different
water. Bees wax link with other materials
environmental conditions. In the methods, Zinc Oxide nanoparticles
were entrapped into wax microspheres using Tween-80 or Tween-20 without any unwanted reactions. sensitive materials such as
as an emulsifier. For evaluating rheology and morphology of nanoparticles are covered with thin layer of wax to
manufacturing capsules can be performed several tests such as using protect from hydrolysis and oxidation. It is used to create
SEM microscopy to proven sphericity of capsules and the size of the a cover around the materials as a hydrophobic layer.
formed capsules, FTIR to prove the sphericity and the wax-zinc oxide In this paper, the synthesis, analysis and
physical bond, XRD spectroscopy to study the presence or absence of
morphologies methods for encapsulation of zinc
nanoparticles without the chemical change in produced capsules and
the efficiency of encapsulation, loading and releasing tests to study oxide nanoparticles are studied.
the value of loaded nanoparticles into microcapsules. According to
tests, the produced capsules are spherical. The Beeswax protects of II. EXPERIMENTAL
Zinc Oxide nanoparticles in undesirable environment and storage
condition. 2.1. The First Method:
Keywords— Beeswax, Encapsulation, Release, ZnO. In this method, the wax (9g) is melted in the beaker by
using a water bath, and then zinc oxide nanoparticles (3g) are
I. INTRODUCTION added to the molten wax. Tween-80 (1.8%w-w) is used
to create a homogeneous emulsions. The
Z INC oxide is a white powder, inorganic and
semiconductor component. It has special properties such
as band gap about 3.37 ev, high continuity energies equal to
entire mixture is stirred for 3-4 minutes at 1000
rpm (using a stirrer RQ -127A) under higher temperature of
wax melting point. In the next step, the temperature of
60 mev, emission near UV wavelength, having piezoelectric
above mixture were brought down quickly, by adding cold
properties and being biocompatible and safe. ZnO nanop
water to temperature 100C.Obtained nano-capsules
articles are important at electrical and
are washed to remove any extra material and they are dried at
telecommunications industries because of
room temperature for 48 h. [1],[2]
their chemical, optical and electrical new properties.
Encapsulation is a new technology to entrap solid, liquid 2.2. The Second Method:
or gas materials into capsules, and to float them in the water.
In this method, certain amount of wax melted in a 900C
The contents of capsule can be controlled under certain
water bath and appropriate amount of ZnO nanoparticles are
conditions by this method.
added. This mixture is poured into 200ml hot aqueous
Encapsulation protects the material from humidity, heat or
mixture containing Tween_20 (1%w-v), and it is mixed with
other conditions. The purpose of this paper is
a stirrer impeller in 1000 rpm for 30 minutes for cooling the
also the encapsulation of ZnO nanoparticles
formed emulsion at room temperature. After filtration, the
by using bees wax to protect it from different
obtained spherical particles washed three times with distilled
environmental conditions and control the release time of
water and they dried at room temperature and passed
nanoparticles. Bees wax was chosen to cover the capsules
through a sieve by 25 number size. [3]
because of its physical and chemical characteristics.
III. CHARACTERIZATION
Roya Namdariyan1 was with Department of Chemical Engineering
shahrood branch, Islamic Azad University, shahrood, Iran, (e-mail: 3.1 The Formation Efficiency of Capsules
[email protected])
Afshin Farahbakhsh2 was with Department of Chemical Engineering,
Efficiency factor of the formation capsule can be used to
Quchan branch, Islamic Azad University, Quchan, Iran, (Corresponding compare different formulations
author’s Phone: +989151892636; e-mail: [email protected]). of synthesis. This parameter is calculated
Hossain Alizade Golestani3 was with Department of Chemical
Engineering,Quchan branch, Islamic Azad University, Quchan, Iran.
and evaluated by measuring the weight of produced
microcapsules and its ratio to the total weight of

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 2nd International Conference on Oil, Gas and Petrochemical Issues(ICOGPI'2013) August 25-26, 2013 Kuala Lumpur (Malaysia)

solid material. For this purpose, produced capsule weighed S = P2 / (12.56 × A) where A is area and P is perimeter.
after drying and the obtained number is divided to the whole
of initial solid material. Thus weight ratio is calculated by 3.3.2. Fourier Transform Infrared Spectroscopy (FTIR)
multiplying this number by 100 and it is as percentage FTIR is a device that can obtain spectral measurements
of the recovery formed capsule that is used to estimate by powders reflection. Infrared spectroscopy is developed by
the efficiency of this process[4].These parameters can be using radiation absorption and vibrating molecules
calculated as follows: and ions. This method is used for measurement
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑐𝑎𝑝𝑠𝑢𝑙𝑒𝑠 and determination the structure of chemical species.
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝑌𝑖𝑒𝑙𝑑 = × 100
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑎𝑙𝑙 𝑠𝑝𝑖𝑐𝑖𝑒𝑠 𝑐ℎ𝑎𝑟𝑔𝑒𝑑 The synthesis experiment was used to prove the strength of the
physical bond between beeswax and zinc oxide.
To identify the effect of encapsulation value on the
3.2. The Encapsulation Efficiency of Nanoparticles
chemical structure of ZnO nanoparticles we obtain FTIR
Another factor for the synthesis of various formulations is spectrum of the empty microcapsules and microcapsules
encapsulation efficiency of the nanoparticles. To achieve containing ZnO nanoparticles and then it compare with the
this criterion, the amount of encapsulated nanoparticles in wax obtained spectra for ZnO pure.
is compared with the amount of used nanoparticles in the
initial times. To access this approach, an appropriate number 3.3.3 X-Ray Diffraction (XRD)
of microspheres are poured into 100 mg phosphate buffer Crystal size can be measured by using both X-ray
mixture (PH = 6.8) and this mixture are put into an ultrasonic diffraction and its collision to the sample. Electromagnet
bath with 700C temperature. After filtration 4ml of suspended spectrum of X-ray is in the range between UV and gamma
solution mixed with 4 ml phosphate buffer mixture (PH = 6.8) radiation. We can obtain information about the sample
to dilute solution by using spectrophotometer. The absorption structure, type of materials and also determination the amount
rate of nanoparticles is measured by a spectrophotometer in of existing elements, by using X-ray. In X- ray diffraction
wavelength of 225 nm. This device, beam falls on the unknown sample from a tube and
measured absorbance amounts indicate the amount of loaded beam’s reflection intensity be measured at different angles.
nanoparticles in microcapsules The main approach in X-ray test is determination the angle
by using calibration curve (a marked related to any peak and the distance of their atomic surface.
plot of absorbance measurements at different concentrations X-ray pattern for each combination is unique and we can
of ZnO nanoparticles by a spectrophotometer). If the amount identify unknown substance with referring to related table. For
of measured weight is multiplied by 100, percent doing this test, peak of pure ZnO nanoparticles, pure wax and
of loaded nanoparticles in produced capsules is microcapsules containing nanoparticles were obtained and
calculated according to this education: compared. Evaluation of the results indicates the presence or
absence of nanoparticles with preserved chemical structure
Encapsulation efficiency% within produced microcapsules.
entrapped amount of ZnO nanoparticles per g capsules
= 3.3.4 Drug Release Test
theorical amount of drug per g capsules
One of the most important properties of encapsulation
3.3. Rheological Studies of Capsules: process is protect the loaded combination through time. Thus
it is necessary to examine how long capsule can prevent
3.3.1. Scanning Electron Microscope (SEM) exiting compound. This study can be assessed by release test
SEM is a zoom tool which the electrons are through time. To evaluate release of ZnO nanoparticles from
used instead of light beams. It is formed capsules, 4 ml phosphate buffer solution is poured in
a research tool in nanotechnology that can provides images cellulose dialysis tube and 100mg of microcapsule would be
of objects as small as 10nm added to the mixture. This tube was rotated at 100rpm in 500
with electron bombarded method, and particles will be studied ml of phosphate buffer solution (pH=6.8) at 370C. A sample
simply with more clarity. Sample bombardment (5ml) was withdrawn at different time with step time of 2 hr
and then an equal volume of fresh buffer is replaced. Then
causes electrons releasing from sample toward the positive
sample is analyzed to obtain ZnO nanoparticles content by
charge surface and all electrons can change into signals. SEM
measuring the absorbance at 254 nm. The concentration of
device can be used in the imaging of formed microcapsules
ZnO nanoparticles are calculated by using calibration curve.
easily. The images obtained by scanning the entire surface Thus the curve of releasing ZnO concentration from the
of microcapsules, can represents the size of capsules versus time can be obtained. The release rate over
produced microcapsules well. time indicates the ability of bees wax to protect loaded
In the other word SEM is an especial tool to measure nanoparticles. We can achieve release rate equation using the
the size of the produced microcapsules and their spherical plot of released ZnO concentration versus time. Thus we
structures. In the usual evaluation methods, surface diameter consider three equations to analyze obtained data and find best
can determine from resulting images and then sphericity factor fitting equation.
is calculated by the equation 5T1. Zero-order release equation [5]: Ft = K0t
5T R R R R

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 2nd International Conference on Oil, Gas and Petrochemical Issues(ICOGPI'2013) August 25-26, 2013 Kuala Lumpur (Malaysia)

2. First-order release equation [6]:

5T 5T Ln(1 − F) = −K1 . t

3. Higuchi equation [7]:

5T F = K 2 . t1/2

Where F represents the fraction of drug release in time t, K 0

4T R R

and K 1 are release rate constant in zero-order and first-order

R R

and K 2 is the Higuchi constant.

R R

IV. CONCLUSION
4T

The Encapsulation ZnO nanoparticles by bees wax

4T

increases persistence time and their release in a controlled

situation. From FTIR studies was investigated there is no
chemical interactions between ZnO nanoparticles and bees
wax. Using suitable surfactants with high HLB value like
Tween-80 and Tween-20 is one of the most important
effective factors in synthesis capsules. Doing structural
examinations along computable factors confirm the accuracy
of capsules synthesis and formation that certainly should be
done in a similar study.

REFERENCES
*
[1] D.V.Gowda, V.K.Gupta , M.Shuaib Khan, A.Batho, “Encapsulation
P P

of Clozapine into Beeswax Microspheres, Preparation, Characterizati

and Release Kinetics”, International Journal of PharmTech Research,
Vol 3, no 4, pp. 2199-2207, Oct-Dec 2011,.
[2] M.Manjunath, A.S.Aravindram, B.Vishvanathan, M.A.Faruqui, D.V
Gowda , M.Shuaib Khan ,”Encapsulation of Olanzapine into Beeswax
Microspheres: Preparation, Characterization and Release Kinetics”,
Latin American Journal of Pharmacy(formerly Acta Farmacéutica
Bonaerense), vol 31, no 6 , pp. 808-14, 2012.
[3] N.Ranjha, H.Khan , S.Naseem , “Encapsulation and characterization
of controlled release flurbiprofen loaded microspheres using beeswax
as an encapsulating agent”, Journal of Materials Science: Materials in
Medicine, , vol 21, no 5, pp.1621-1630 ). May 2010.
[4] Y.Samati, N.Yuksel, N.Tarimci.” Preparation and characterization of
poly (D, L-lactic-co-glycolic Acid) microspheres containing
flurbiprofen sodium.Drug Deliv”, pp.13:105-11, 2011.
[5] N.Najib, M.Suleiman.“The kinetics of drug release from ethylcellulose
solid dispersion Drug Dev Ind pharm”., pp.11:2169-89, 1985.
[6] S.Desai, P.Singh, A.P.Simonelli, WL Higuchi. “Investigation of
factors influencing release of solid drug dispersed in inert matrices. II.
Quantitative studies involvin polyethylene plastic matrix.” J Pharm Sci.
pp.55:1230–4, 1966.
[7] T.Higuchi. “Mechanism of sustained action medication: theoretical
analysis of rate of release of solid drugs dispersed in solid matrix”. J
Pharm Sci. pp.50:1145–9, 1963.

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