A New detection method of flavors and fragrances microcapsules release property

Abstract

The invention discloses a method for detecting the release performance of flavors and fragrances microcapsule, comprising the following steps: Using SPME to adsorb the gas sample released by the perfume microcapsules in different time periods under constant temperature and humidity conditions. The SPME adsorption time was 10 s30 min and the analytical time in GC/MS was is 1 s100 min, and the compounds detected by GC-MS were quantified by area normalization method. The method of the invention is simple and rapid, and is suitable for analyzing and detecting the sustained release of the perfume microcapsules. Using SPME technology, the detection process was without the use of organic solvents and green pollution. The invention can be directly used for the detection of the release of gas components of various perfume microcapsule products without destroying the sample morphology and structure, and more truly reflecting the release performance of the flavors and fragrances microcapsule in real life.

Claims

1. The invention relates to a method for detecting the release property of a perfume fragrance microcapsule, which comprises the following steps: Using SPME to adsorb the gas sample released by the perfume microcapsules in different time periods under constant temperature and humidity conditions. The SPME adsorption time was 10 s30 min and the analytical time in GC/MS was 1 s100 min, and the compounds detected by GC-MS were quantified by area normalization method.

2. The detection method according to claim 1, the SPME coating is one of PDMS, PDMS/DVB, PDMS/DVB/CAR and PA.

3. The detection method according to claim 1, the different time periods are the 1st, 3rd, 5th, 7th, 9th, 17th, 20th, 24th, 27th in a month.

4. The detection method according to claim 1, the adsorption time for the gas sample for the perfume microcapsules in different time periods by SPME is 1 to 24 hours.

5. The detection method according to claim 1, the gas is adsorbed by SPME under constant temperature condition for different time periods, and the constant temperature and humidity range is: temperature 10 C. to 90 C. and humidity 595%.

6. The detection method according to claim 1, the conditions of the GC-MS are SHIMADZU GC/MS-QP2010 Plus gas chromatography-mass spectrometer and a Rtx-5MS capillary column (30.0 m0.25 um250 mm), and the carrier gas is high purity helium flow rate 3.0 mL/min; program temperature: the initial temperature of 40 C. keeping in 1 min and raising ire 10 C./min to 230 C. keeping for 5 min. The split ratio was 50:1 and ion source temperature was 240 C. The ionization mode was EI and scanning mass range 35 m/z-500 m/z.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0018] FIG. 1 shows the total ion chromatogram of the release of the gas component of the lavender essential oil microcapsule;

[0019] 1-tartin; 2-foliage; 3-linalool; 4-camphor; 5-terpinen-4-ol; 6-acetic acid camphor vinegar; 7-acetic acid lavender vinegar; 8--terpilenol

[0020] FIG. 2 for the lavender microcapsules at 30 C., 60% humidity sealed for 30 days sustained release effect map;

[0021] FIG. 3 for the lavender microcapsules at 30 C., 80% humidity sealed 20 days sustained release effect map;

[0022] FIG. 4 for the lavender microcapsules at 30 C., 8% humidity sealed 20 days sustained release effect map;

[0023] FIG. 5 for the detection flow chart.

DETAILED DESCRIPTION OF THE INVENTION

[0024] The present invention will be further described with reference to the following examples, but the scope of protection of the present method is not limited to the scope of the embodiments.

Example 1

[0025] Lavender essential oil microcapsules were tested in release performance. 0.010 g of lavender essential oil microcapsule samples were placed in a 20.0 mL headspace bottle. On the first day, GC-MS was analyzed by CAR-DVB-PDMS (50/30) coated SPME for 1 hour after the release of gas for 1 h at a constant temperature of 30 C. and a humidity of 60%

[0026] Day 2, constant temperature and humidity box was emptied the bottle and opened vent, place time 1 day.

[0027] On the third day, the gas s extracted with CAR/DVB/PDMS (50/30) and take 1 h for GC-MS analysis.

[0028] Day 4 emptied bottle and opened vent in constant temperature and humidity box, place fort day.

[0029] Day 5, the gas was extracted with CAR/DVB/PDMS (50/30) coated SPME for 1 h, and analyzed by GC-MS.

[0030] And so on, the 6 days, 7 days, 8 days . . . to 27 days.

[0031] GC-MS test conditions are all the same: the conditions of the GC-MS are SHIMADZU GC/MS-QP2010 Plus gas chromatography-mass spectrometer and a Rtx-5MS capillary column (30.0 m0.25 0.25 um250 mm), and the carrier gas is high purity helium flow rate 3.0 mL/min; program temperature: the initial temperature of 40 C. keeping in 1 min and raising in 10 C./min to 230 C. keeping for 5 min. The split ratio was 50:1 and ion source temperature was 240 C. The ionization mode was EI and scanning mass range 35 m/z-500 m/z.

[0032] Slow release effect as shown in FIG. 2, the daily slow release volume decreases with time, the data fitting analysis, the microcapsule sustained release model in line with the release model, the fitting curve: Y=exp(0.9037x+20.3419), R2=0.99681

Example 2

[0033] Lavender essential oil microcapsules were tested in a sustained-release performance, and 0.010 g of lavender essential oil microcapsule samples were placed in a 20.0 mL headspace bottle. On the first day, the cells were allowed to stand for 24 hours at a constant temperature of 30 C. and a humidity of 80%. After 24 days, the gas was extracted with CAR/DVB/PDMS (50/30) GC-MS analysis.

[0034] Day 3, emptied bottle and opened vent in constant temperature and humidity box, place for 1 day.

[0035] Day 4, the gas was extracted with CAR/DVB/PDMS (50/30) coating SPME on the release of gas and take 1 h for GC-MS analysis.

[0036] Day 5, constant temperature and humidity box top empty bottle open vent, place time 2 days.

[0037] Day 7, the gas was extracted with CAR-DVB-PDMS (50/30) coating SPME on the gas and take 1 h for GC-MS analysis.

[0038] And so on, the first 8 days, 9 days, 11 days . . . to the 19th day. GC-MS test conditions are all the same: the conditions of the GC-MS are SHIMADZU GC/MS-QP2010 Plus gas chromatography-mass spectrometer and a Rtx-5MS capillary column (30.0 m0.25 um250 mm), and the, carrier gas is high purity helium flow rate 3.0 mL/min; program temperature: the initial temperature of 40 C. keeping in 1 min and raising in 10 C./min to 230 C. keeping for 5 min. The split ratio was 50:1 and ion source temperature was 240 C. The ionization mode was EI and scanning mass range 35 m/z-500 m/z.

[0039] Slow release effect diagram shown in FIG. 3, the daily slow release volume decreases with time, the data fitting analysis, the microcapsule sustained release model in line with the first release model the curve is: Y=exp (3255x+18.3259), R2=0.98683

Example 3

[0040] Lavender essential oil microcapsules were tested in a sustained-release performance, and 0.010 g of lavender essential oil microcapsule samples were placed in a 20.0 mL headspace bottle. On the first day, the cells were sealed with a CAR/DVB/PDMS (50/30) coating SPME for 1 h. and the gas was extracted for 1 h after release for 47 h at a constant temperature of 30 C. and a constant humidity of 80%-MS analysis.

[0041] On the third day, the top empty bottle in the constant temperature and humidity chamber was ventilated and placed for 47 hours. The gas was extracted with CAR/DVB/PDMS (50/30) coating SPME for 1 h, and GC-MS analysis.

[0042] Day 5, constant temperature and humidity box top empty bottle open vent, place the time 71 h after sealing the top empty bottle. GC/MS analysis was carried out using CAR/DVB/PDMS (50/30) coated SPME for 1 h after the release of the gas.

[0043] Days 7, constant temperature and humidity box top empty bottle open vent, place the time after 23 h sealed the top empty bottle. GC/MS analysis was carried out using CAR/DVB/PDMS (50/30) coated SPME for 1 h after the release of the gas.

[0044] Day 8, constant temperature and humidity box top empty bottle open vent, place the time after 23 h sealed top empty bottle. GC/MS analysis was carried out using CAR/DVB/PDMS (50/30) coated SPME for 1 h after the release of the gas.

[0045] And so on, the first 9 days, 10 days, 11 days . . . to the 19th day.

[0046] GC-MS test conditions are all the same: the conditions of the GC-MS are SHIMADZU GC/MS-QP2010 Plus gas chromatography-mass spectrometer and a Rtx-5MS capillary column (30.0 m0.25 um250 mm), and the carrier gas is high purity helium flow rate 3.0 mL/min; program temperature: the initial temperature of 40 C. keeping in 1 min and raising in 10 C./min to 230 C. keeping for 5 min. The split ratio was 50:1 and ion source temperature was 240 C. The ionization mode was, EI and scanning mass range 35 m/z-500 m/z.

[0047] Sustained release effect diagram shown in FIG. 4, the instantaneous release of microcapsules with the amount of time to reduce the length of the data. The results showed that the sustainedrelease model of microcapsules was in accordance with the firstorder release model. The fitting curve was Y=exp(0.2069x+17.0337) and R2=0.94444.