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Pol. J.10.1515/pjct-2017-0013
Chem. Tech., Vol. 19, No. 1, 2017 89
Micro-encapsulated strawberry fragrance was successfully prepared with wall materials including maltodextrin, sodium
octenylsuccinate and gum Arabic. The micro-capsule was added to wallpaper and aromatic wallpaper with strawberry
characteristics was obtained. The particle distribution, surface morphology, chemical structure, thermal property
and controlled release performance of micro-encapsulated fragrance and aromatic wallpaper were investigated
using laser particle size analyzer, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy
(FT-TR), thermal gravity analysis (TGA) and chromatography-mass spectrometer (GC-MS). The results showed
that the average diameter of micro-capsule was 2 μm and the particles mainly distributed in the tissues of wallpaper.
The result of TGA showed that the micro-capsule had a good stability. Meanwhile, the aromatic wallpaper had
strawberry aroma more than 3 months and took on excellent controlled release performance.
EXPERIMENTS
Materials
Maltodextrin (DE degree: 10–15) was purchased from
Dongxiao Biological Technology Co. Ltd (Shandong
zhucheng, China). Purity gum 2000 came from National
Starch Co. Ltd (Shanghai, China). Gum Arabic (AR)
was obtained from Aladdin Biological Technology Co.
Ltd (Shanghai, China). Styrene-butadiene latex and wal-
lpaper were provided by Qifeng Specialty Paper Co. Ltd
(Shandong, China). Strawberry fragrance and deionized
water were prepared by our lab.
port of GC-MS and the time of sample injection susta- fibers constituted the wallpaper. After the aromatic tre-
ined for 5 min. atment, micro-capsules were glued at the wood fibers of
The conditions of head-space solid phase-micro-extrac- wallpaper. The size of particles stuck at the wood fibers
tion were as follows: the aging temperature of extraction was in accord with the result of particle size distribution
was 250oC. The extraction fiber was aged for 20 min in analysis. All these results demonstrated the successful
N2 flow at the rate of 1.0 mL/min. preparation of micro-capsules and aromatic wallpaper.
The condition of gas chromatography-mass spectro-
metry was as follows: the chromatographic column was FT-IR ANALYSIS
DB-Innowax capillary column (60 m × 0.25 mm × 0.25
μm, Agilent). Helium (purity = 99.999%) was selected Figure 4 shows the infrared spectrograms of micro-
as carrier gas at a rate of 2.0 mL/min. Column oven -encapsulated strawberry fragrance, blank wallpaper,
adopted temperature programming. Firstly, it started micro-encapsulated strawberry aromatic wallpaper and
at 40oC maintaining for 6 min. Secondly, the empera- strawberry fragrance. Compared with strawberry fra-
ture rose at the rate of 3oC/min to 100oC. And then, grance and micro-encapsulated strawberry fragrance,
the temperature rose at the rate of 5oC/min to 230oC 5 characteristic absorption peaks had relatively large
keeping for 10 min. Electron bombardment ion source changes (namely: the stretching vibration absorption
was used. The electron energy was 70 eV. The spectra peak at 3396 cm–1 of O-H bond, the stretching vibra-
collection mode was full scanning at the range of 30–450 tion at 2925 cm–1 of C-H bond in the group of -CH2-23,
amu. The solvent delayed for 3.00 min. the stretching vibration at 1737 cm–1 of C=O bond in
The qualitative and quantitative determination me- the carboxylic acid or esters, the stretching vibration
thod of chemical compound was as follows: The mass at 1226 cm–1 of C-O bond in esters and the stretching
spectrums of unknown compounds were compared with vibration at 1031 cm–1 of C-X bond). From the spec-
the spectrum libraries of NIST and WILEY 7n (Agilent trograms of micro-encapsulated fragrance and normal
Technologies Inc.). The content of each compound was fragrance in Figure 4, the changes in the absorption
calculated by area normalization method of peak area. strength were observed. The absorption strength of
strawberry micro-encapsulated fragrance was stronger
than that of the normal strawberry fragrance. Owing
RESULTS AND DISCUSSION
to the coating action of wall material towards the core
material, the infrared absorption of strawberry fragrance
Particle size distribution and morphology analysis was obstructed. Therefore, weak absorption strength of
The micro-capsule liquid prepared above was put micro-encapsulated strawberry fragrance was observed.
into the sample cell for particle size distribution analy- Furthermore, other changes such as the disappearing,
sis. It was repeated three times. Figure 2 represented bath chromic shift and hypo chromatic shift were also
the results. As for the whole particle size distribution observed. For example, the absorption peak at 1737 cm–1
shape, a normal distribution can be observed. Particle of C=O bond in aldehydes materials disappeared; the
size distribution ranged from 1 μm to 2.5 μm. And the absorption peak at 2925 cm–1 moved into 2936 cm–1.
mean diameter of micro-capsule was 2 um. A narrow All of these changes were caused by the interaction
unimodal distribution demonstrated that the system was between the wood fibers and the micro-encapsulated
stable and homogeneous22. Figure 3 was the scanning fragrance. Hence, these results indirectly testified the
electron microscope photos of blank wallpaper and strawberry fragrance was successfully embedded in the
micro-encapsulated aromatic wallpaper at the same cavity of micro-capsule. The difference was not obvious
magnification times. The micro-structure of wallpaper between the infrared spectrograms of blank wallpaper
can be seen from Figure 3. A series of disorderly wood and micro-encapsulated aromatic wallpaper as Figure 4.
The fragrance has a strong odor in spite of low dose.
In consideration of the trait of fragrance, only 1% of
micro-encapsulated fragrance was added into the wall- occurred due to the lost of free water and fragrance
paper. So, the biggest difference between the wallpaper absorbing at the surface of micro-capsules. Secondly, the
and micro-encapsulated aromatic wallpaper was odor thermal decomposition was at the range of 240–600oC.
rather than the chemical structure. Therefore, the con- Two stages consisted of this phase. The formal stage was
sequence of an unambiguous distinction between blank corresponding to the rapid release of the core material
wallpaper and micro-encapsulated aromatic wallpaper with the maximum decomposition rate at 282.5oC. The
was observed. The wallpaper was macromolecular poly- maximum decomposition rate appeared at 307.84oC of
saccharide cellulose and its structural unit was glucose. the latter stage which caused by the decomposition of
Therefore, some of the absorption peaks of wallpaper wall material. In consequence of embedding of the wall
existed in the range of 1200 cm–1 to 950 cm–1 24, such material, the maximum volatile rate temperature of core
as absorption peaks at 1178 cm–1, 1059 cm–1 and 1039 material changed from 112.9oC to 282.5oC. However, with
cm–1. For aroma wallpaper, the absorption peaks at the temperature increase, the core material in the cavity
3376 cm–1, 2964 cm–1 and 1178 cm–1 were all moved to brought about the increase of vapor pressure. The vapor
the direction of the long wave. It was the direction of pressure made the gap existing in the surface of micro-
characteristic absorption peaks of micro-encapsulated -capsule bigger than before, and thus, the core material
fragrance. These appearances manifested that micro- quickly leaked from the micro-capsule cavity26. Compared
-encapsulated fragrance was absorbed in wallpaper. The with the thermal decomposition curves of strawberry fra-
strength of the absorption peak at 3376 cm–1 was because grance and micro-encapsulated strawberry fragrance, we
of the overlay of absorption peak of micro-encapsulated knew that the micro-encapsulated strawberry fragrance
fragrance. The absorption peaks of stretching vibration possessed good thermal stability. This guaranteed the
at 1737 cm–1 in wallpaper, stretching vibration at 1059 stability of the micro-encapsulated strawberry fragrance
cm–1 of C-X bond in wallpaper, stretching vibration at in the application of aromatic wallpaper.
1039 cm–1 of C-O-C of the pyranoid ring of wallpaper
were not changed in position and strength25. This indi- GC-MS analysis of the controlled release of aromatic
cated that the chemical structure of wallpaper was not wallpaper
changed. And the aromatic treatment of wallpaper was Controlled release of micro-encapsulated fragrance
worked relying on the hydrogen bonds or the van der is an important parameter to confirm the effect of mi-
Waals forces of intermolecular physical interaction. cro-encapsulation. The micro-encapsulated strawberry
fragrance was added in wallpaper. The obtained aro-
TG analysis matic wallpaper was expected to have controlled and
Figure 5 shows the thermogravimetric curves of straw- sustained release pleasure odor. Figure 6 shows the
berry fragrance, strawberry micro-encapsulated fragrance results of aroma content changes with the increase of
and blank micro-encapsulated wall material respectively. storage time for two type aromatic wallpaper. From the
From Figure 5a, it can be seen that the mass of straw- Figure 6, we knew that the aroma content of aromatic
berry fragrance was gradually lost with the increase of wallpaper appeared continuous reduction from 0 to 90
temperature and the majority of mass lost at the scope days. The fragrance is easily volatile. After the homoge-
of 60–140oC. The maximum thermal decomposition speed neous coating at the wallpaper via physical interaction,
happened at 112.9oC. When the temperature rose to the strawberry fragrance was rapidly volatilized with
200oC, strawberry fragrance was volatilized completely the bigger contact area between the fragrance and air.
and there was no remnant. From Figure 5b and Figure Therefore, in the initial phase, the aroma content of
5c, three steps of thermal decomposition for strawberry the aromatic wallpaper was bigger than the micro-en-
micro-encapsulated fragrance and blank micro-capsule capsulated aromatic wallpaper’ in spite of at the same
can be observed. First of all, it took place below 250oC. fragrance adding amount. However, with the increase of
In this phase, strawberry micro-encapsulated fragrance time, the amount of residual fragrance in the aromatic
lost 6.35% while the blank micro-capsule lost 8.23% wallpaper was less and less. At 40 days, no fragrance
in mass. The thermal decomposition of this step was
Figure 5. TG curves of fragrance (a), microencapsulated fra- Figure 6. Fragrance release curves of aromatic wallpaper and
Unauthenticated
grance (b) and blank microcapsule (c) microencapsulated aromatic wallpaper
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Pol. J. Chem. Tech., Vol. 19, No. 1, 2017 93
in the aromatic wallpaper can be detected by GC-MS. essential oils microcapsules based on complex coacervation
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ACKNOWLEDGMENTS 14. Zhao, H.M., Chen, X. & Wu, J. (2001). The preparation,
This work was financially supported by the National properties and using of starch sodium alkenylsuccinate. Cereal
Key R&D Program (2016YFA0200300), Shanghai Plateau Food Ind. 1, 23–27. DOI: 10.3969/j.issn.1672-5026.2002.01.008.
15. Hu, L. (2010). Study on the mciroencapsulation of fish oil
Discipline “Chemical Engineering and Technology (Per-
using Chitosan/ Gum acacia complex coacervation method. Ma-
fume and Aroma Technology) and the National Natural ster dissertation, Ocean University of China, Shangdong, China.
Science Fund of China (No. 21276157, No. 21476140). 16. Ge, X., Fei, X. Q., Chen, Y., Luo, F. & Wang, Y.P.
(2013). Properties of oil-tea camellia seed oil microcapsule
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1. Xiao, Z., Liu, W., Zhu, G., Zhou, R. & Niu, Y. (2014).
A review of the preparation and application of flavour and Unauthenticated
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