CN112505164A - Method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics - Google Patents
Method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics Download PDFInfo
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- CN112505164A CN112505164A CN202010666978.7A CN202010666978A CN112505164A CN 112505164 A CN112505164 A CN 112505164A CN 202010666978 A CN202010666978 A CN 202010666978A CN 112505164 A CN112505164 A CN 112505164A
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 title claims abstract description 54
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 52
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 title claims abstract description 36
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000002537 cosmetic Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- 229960000541 cetyl alcohol Drugs 0.000 title claims abstract description 19
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 title claims abstract description 18
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 title claims description 20
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 title claims description 14
- 229940051250 hexylene glycol Drugs 0.000 title claims description 10
- 239000012086 standard solution Substances 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012224 working solution Substances 0.000 claims abstract description 11
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004817 gas chromatography Methods 0.000 claims abstract description 6
- 239000012488 sample solution Substances 0.000 claims abstract description 5
- 229920005862 polyol Polymers 0.000 claims description 39
- 150000003077 polyols Chemical class 0.000 claims description 39
- 239000000523 sample Substances 0.000 claims description 21
- 239000011550 stock solution Substances 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000012937 correction Methods 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims 5
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 abstract description 8
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 abstract description 6
- 150000005846 sugar alcohols Polymers 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004909 Moisturizer Substances 0.000 description 2
- 235000019437 butane-1,3-diol Nutrition 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000001333 moisturizer Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Cosmetics (AREA)
Abstract
The invention provides a method for measuring propylene glycol, butanediol, hexanediol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics, which mainly comprises three main steps of preparing an internal standard solution by using isooctyl alcohol and absolute ethyl alcohol, preparing a working solution by using the internal standard solution and polyhydric alcohol and carrying out gas chromatography measurement on a sample solution to be measured.
Description
Technical Field
The invention relates to the field of cosmetic detection methods, in particular to a method for detecting propylene glycol, butanediol, hexanediol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics.
Background
At present, the content of seven polyols, namely propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol, in cosmetics is very high, and polyol humectants in cosmetics mainly comprise seven polyols, namely propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol, and although the polyol moisturizers have good moisturizing effects, excessive use of the polyol moisturizers also has potential hazards. Exposure to high concentrations can cause serious health damage, resulting in damage to the central nervous system and various organs. At present, detection methods and documents for simultaneously testing the content of seven polyols, namely propylene glycol, butanediol, hexanediol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol, in cosmetics are not available, and research and establishment of a method for simultaneously determining the polyol in the cosmetics are necessary.
The invention provides a method for measuring propylene glycol, butanediol, hexanediol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics, establishes a method for simultaneously measuring 7 polyols in the cosmetics by using a gas chromatograph for the first time, supplements the method for measuring the polyols in the cosmetics, determines an extraction reagent and ultrasonic time required in an experiment, and determines chromatographic conditions.
Disclosure of Invention
The invention provides a method for measuring propylene glycol, butanediol, hexanediol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics, which comprises the following specific scheme:
a method for measuring propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics is characterized in that the measuring method comprises the following steps:
s1: preparing internal standard solution with isooctanol concentration of 0.2% by using isooctanol and absolute alcohol for later use;
s2: preparing a polyol working solution with the polyol concentration of 0.5% by using the internal standard solution and the polyol for later use;
s3: injecting a polyol working solution according to the selected chromatographic conditions, and calculating a polyol relative correction factor RRFi by using the following formula:
RRFi＝(CST*AIS)/(AST*CIS)
wherein CST is the concentration (%) of the standard solution, AST is the peak area of the standard, AIS is the peak area of the internal standard solution, and CIS is the concentration (%, v/v) of the internal standard solution;
s4: dissolving a sample to be detected in an internal standard solution;
s5: extracting the supernatant in the sample solution, and measuring by using gas chromatography;
s6: the content of each alcohol was calculated according to the following formula:
Xi％＝RRFi*[(CIS*AXI)/(CSA*AIS)]*100％
wherein Xi is the percentage content of the alcohol to be measured, CIS is the concentration of the internal standard solution, CSA is the sample concentration, AXI is the peak area of the alcohol to be measured, and AIS is the peak area of the internal standard.
Further, the step of preparing the polyol working solution in step S2 includes the following steps:
s21: preparing a polyol stock solution having a polyol concentration of X-Y% using a polyol and the internal standard solution prepared in step S1;
s22: the internal standard solution prepared in step S1 was added again to the polyol stock solution prepared in step S21 to prepare a polyol working solution having a polyol concentration of 0.05% (not filled in here).
Further, the internal standard solution prepared in step S1 preferably has an isooctanol concentration of 0.2%.
Further, in step S4, the preferable mode for dissolving the sample to be tested is as follows:
s41: selecting 0.5g of sample and placing the sample in a 100ml triangular flask;
s42: 10.0ml of internal standard solution is added into a triangular flask and shaken for 20 min.
Further, in the step S5, the manner of extracting the supernatant in the sample solution is preferably to place the internal standard solution of the sample to be tested in a centrifuge tube, and centrifuge at 8500r/min for 20 min.
Drawings
FIG. 1 is a gas chromatogram of seven detected elements according to an embodiment of the present invention. 1-isooctanol, 2-propanediol, 3-butanediol, 4-lauryl alcohol, 5-hexanediol, 6-glycerol, 7-cetyl alcohol, 8-stearyl alcohol.
Detailed Description
The invention can be used for detecting propylene glycol, butanediol, hexanediol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics, and can be detected in laboratories carrying out gas chromatography detection. The detection method provided by the invention has the advantages that the Relative Standard Deviation (RSD) is less than 5%, and the accuracy is higher.
In one embodiment of the invention, the reagents and purities required are as follows:
| name of reagent | Purity of |
| Propylene glycol | ≥98％ |
| Glycerol | ≥98％ |
| 1, 3-butanediol | ≥98％ |
| Hexanediol | ≥98％ |
| Lauryl alcohol | ≥98％ |
| Cetyl alcohol | ≥98％ |
| Stearyl alcohol | ≥98％ |
| Anhydrous ethanol | Super grade pure |
| Isooctyl alcohol | Analytically pure, the purity is more than or equal to 98 percent |
In one embodiment of the present invention, the required instrumentation is as follows:
wherein, the requirements on the gas chromatography conditions are as follows:
a chromatographic column: HP-20M capillary column 50M × 0.32mm × 0.5 μ M (film thickness)
Carrier gas: n is a radical of2The purity is more than or equal to 99.999 percent
Gas combustion: h2The purity is more than or equal to 99.999 percent
Combustion-supporting gas: air (a)
Sample inlet temperature: 250 deg.C
Detector temperature: 260 deg.C
And (3) sample introduction mode: split ratio of 1: 30 split sample injection
Flow rate of carrier gas: 1.0ml/min
The temperature rising procedure is as follows: heating to 190 deg.C at 120 deg.C/min, heating to 220 deg.C at 20 deg.C/min, and holding for 15min
The sample size is 1 mu L
Before detection, 0.2ml of isooctanol is transferred into a 100ml volumetric flask, dissolved by absolute alcohol, diluted to a scale and shaken up for storage, so as to prepare the internal standard solution.
Accurately weighing 0.500g of polyhydric alcohol in 100ml volumetric flasks respectively, dissolving with the internal standard solution, fixing the volume to the scale, and mixing uniformly. The polyol concentrations in the baths were 0.500%, respectively, to prepare polyol stock solutions.
Respectively transferring 5ml of the stock solution into a 50ml volumetric flask, diluting the stock solution to a scale by using an internal standard solution, and uniformly mixing. The concentrations of the polyhydric alcohols in the solutions were 0.05%, respectively, to thereby prepare polyhydric alcohol working solutions.
Before the sample to be detected is detected, a polyol working solution is used for calculating a correction factor RRF under the selected chromatographic conditionsi。
RRFi＝(CST*AIS)/(AST*CIS)
Wherein, CSTAs standard solution concentration (%), ASTIs the standard peak area, AISIs the peak area of the internal standard solution, CISThe concentration of the internal standard solution (%, v/v).
Determining a correction factor RRFiThereafter, the instrument can be turned on normally as required for operation. After the experimental instrument is started, the sensitivity, stability and separation efficiency of the instrument are firstly checked, so that all the detection instruments reach the optimal state under the existing conditions.
Accurately weighing about 0.500g of a sample to be detected into a 100ml triangular flask, adding 10.0ml of internal standard solution, and shaking for 20min to fully mix the sample to be detected and the internal standard solution. The extract was then transferred to a centrifuge tube and centrifuged at 8500 rpm for 20 min. After centrifugation, the supernatant in the centrifuge tube was selected and quantified using an internal standard method as a liquid for measurement by a gas chromatograph. In the test experiment, if the peak shape of the internal standard substance in the sample to be tested is abnormal, the external standard method is used for quantitative re-analysis instead.
When the content of each alcohol in a sample to be measured is measured by gas chromatography, the operation and recording of test data should be performed in accordance with the operation method described in the gas chromatograph manual.
By using the test method, the detection limit of seven polyols can be obviously reduced, and the recovery rate is improved. The detection limits and recovery rates in this example are shown in the following table:
| name of article | Determination Low Limit (%) | Recovery (%) |
| Propylene glycol | 0.02 | 104.5 |
| 1, 3-butanediol | 0.02 | 91.0 |
| Hexanediol | 0.02 | 105.0 |
| Lauryl alcohol | 0.01 | 104.0 |
| Glycerol | 0.5 | 99.8 |
| Cetyl alcohol | 0.02 | 98.0 |
| Stearyl alcohol | 0.02 | 104.0 |
In this example, the gas chromatogram of the detected polyol is shown in FIG. 1. The names and retention times of the individual polyols in the figure are as follows:
the general data acquisition control system provided by the invention is described in detail, and the principle and the implementation mode of the invention are explained by applying specific examples, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and the content of the present specification should not be construed as a limitation to the technical solution of the present invention.
Claims (5)
1. A method for measuring propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics is characterized in that the measuring method comprises the following steps:
s1: preparing internal standard solution with isooctanol concentration of 0.2% by using isooctanol and absolute alcohol for later use;
s2: preparing a polyol working solution with the polyol concentration of 0.5% by using the internal standard solution and the polyol for later use;
s3: injecting a polyol working solution according to the selected chromatographic conditions, and calculating a polyol relative correction factor RRFi by using the following formula:
RRFi＝(CST*AIS)/(AST*CIS)
wherein, CSTAs standard solution concentration (%), ASTIs the standard peak area, AISIs the peak area of the internal standard solution, CISIs insideConcentration of standard solution (%, v/v);
s4: dissolving a sample to be detected in an internal standard solution;
s5: extracting the supernatant in the sample solution, and measuring by using gas chromatography;
s6: the content of each alcohol was calculated according to the following formula:
Xi％＝RRFi*[(CIS*AXI)/(CSA*AIS)]*100％
wherein, XiAs a percentage of alcohol to be measured, CISConcentration of the internal standard solution, CSAAs sample concentration, AXIThe peak area of the alcohol to be measured, AISPeak area of the internal standard.
2. The method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerin, stearyl alcohol and cetyl alcohol in cosmetics according to claim 1, wherein the step of preparing the polyol working solution in the step S2 comprises the steps of:
s21: preparing a polyol stock solution having a polyol concentration of 0.5% using a polyol and the internal standard solution prepared in step S1;
s22: the internal standard solution prepared in step S1 was added again to the polyol stock solution prepared in step S21 to prepare a polyol working solution having a polyol concentration of 0.05%.
3. The method for measuring propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerin, stearyl alcohol, and cetyl alcohol in a cosmetic according to claim 1, wherein the concentration of the internal standard solution, preferably isooctyl alcohol, prepared in step S1 is 0.2%.
4. The method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerin, stearyl alcohol, and cetyl alcohol in a cosmetic according to claim 1, wherein the preferable manner of dissolving the sample to be tested in step S4 is:
s41: selecting 0.5g of sample and placing the sample in a 100ml triangular flask;
s42: 10.0ml of internal standard solution is added into a triangular flask and shaken for 20 min.
5. The method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics according to claim 1, wherein the manner of extracting the supernatant in the sample solution in step S5 is preferably to place the internal standard solution of the sample to be tested in a centrifuge tube and centrifuge at 8500r/min for 20 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010666978.7A CN112505164A (en) | 2020-07-10 | 2020-07-10 | Method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010666978.7A CN112505164A (en) | 2020-07-10 | 2020-07-10 | Method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics |
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| CN112505164A true CN112505164A (en) | 2021-03-16 |
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| CN202010666978.7A Pending CN112505164A (en) | 2020-07-10 | 2020-07-10 | Method for determining propylene glycol, butylene glycol, hexylene glycol, lauryl alcohol, glycerol, stearyl alcohol and cetyl alcohol in cosmetics |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104345096A (en) * | 2013-07-31 | 2015-02-11 | 伽蓝（集团）股份有限公司 | Method for rapidly detecting polyols in cosmetic |
| CN106018620A (en) * | 2016-07-04 | 2016-10-12 | 华南理工大学 | Method for quickly and accurately detecting formaldehyde content and methanol content in cosmetics |
| CN108828123A (en) * | 2018-06-26 | 2018-11-16 | 安徽皖维高新材料股份有限公司 | A kind of method of butyraldehyde and para-acetaldehyde content in measurement polyvinyl butyral resin |
| US20190227011A1 (en) * | 2016-06-28 | 2019-07-25 | Ocean University Of China | Method for measuring sterol content by utilizing quantitative nuclear magnetic resonance technology |
| CN110954632A (en) * | 2019-12-30 | 2020-04-03 | 广州艾蓓生物科技有限公司 | Method for determining content of 1,2-hexanediol in cosmetics |
-
2020
- 2020-07-10 CN CN202010666978.7A patent/CN112505164A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104345096A (en) * | 2013-07-31 | 2015-02-11 | 伽蓝（集团）股份有限公司 | Method for rapidly detecting polyols in cosmetic |
| US20190227011A1 (en) * | 2016-06-28 | 2019-07-25 | Ocean University Of China | Method for measuring sterol content by utilizing quantitative nuclear magnetic resonance technology |
| CN106018620A (en) * | 2016-07-04 | 2016-10-12 | 华南理工大学 | Method for quickly and accurately detecting formaldehyde content and methanol content in cosmetics |
| CN108828123A (en) * | 2018-06-26 | 2018-11-16 | 安徽皖维高新材料股份有限公司 | A kind of method of butyraldehyde and para-acetaldehyde content in measurement polyvinyl butyral resin |
| CN110954632A (en) * | 2019-12-30 | 2020-04-03 | 广州艾蓓生物科技有限公司 | Method for determining content of 1,2-hexanediol in cosmetics |
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| Title |
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Application publication date: 20210316 |