CN112526052A - Method for measuring caprylyl glycol in cosmetic preservative by gas chromatography - Google Patents
Method for measuring caprylyl glycol in cosmetic preservative by gas chromatography Download PDFInfo
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- CN112526052A CN112526052A CN202011528331.4A CN202011528331A CN112526052A CN 112526052 A CN112526052 A CN 112526052A CN 202011528331 A CN202011528331 A CN 202011528331A CN 112526052 A CN112526052 A CN 112526052A
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- AEIJTFQOBWATKX-UHFFFAOYSA-N octane-1,2-diol Chemical compound CCCCCCC(O)CO AEIJTFQOBWATKX-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000003755 preservative agent Substances 0.000 title claims abstract description 40
- 230000002335 preservative effect Effects 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002537 cosmetic Substances 0.000 title claims abstract description 22
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000003965 capillary gas chromatography Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011550 stock solution Substances 0.000 claims abstract description 10
- 239000012086 standard solution Substances 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000007865 diluting Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 5
- -1 octyl glycol Chemical compound 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000002737 fuel gas Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000003908 quality control method Methods 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- GHBFNMLVSPCDGN-UHFFFAOYSA-N rac-1-monooctanoylglycerol Chemical compound CCCCCCCC(=O)OCC(O)CO GHBFNMLVSPCDGN-UHFFFAOYSA-N 0.000 description 2
- 208000002874 Acne Vulgaris Diseases 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 206010000496 acne Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229940087068 glyceryl caprylate Drugs 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- WCVRQHFDJLLWFE-UHFFFAOYSA-N pentane-1,2-diol Chemical compound CCCC(O)CO WCVRQHFDJLLWFE-UHFFFAOYSA-N 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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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)
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Abstract
The invention discloses a method for measuring caprylyl glycol in a cosmetic preservative by gas chromatography, which comprises the following steps: (1) preparing a standard octyl glycol stock solution; (2) preparing the octyl glycol standard stock solution into a series of standard solutions with different concentrations of 15-300g/L by using absolute ethyl alcohol; (3) measuring the series of standard liquids with different concentrations by adopting a capillary gas chromatography, and performing linear fitting by taking the peak area of the series of standard liquids as a horizontal coordinate x and the concentration as a vertical coordinate y to obtain a standard curve with a correlation coefficient larger than 0.999; (4) weighing a preservative sample, diluting and dissolving the preservative sample by absolute ethyl alcohol to obtain a sample detection solution, detecting the sample detection solution under the condition of capillary gas chromatography, and calculating according to a peak area to obtain the content of the caprylyl glycol. The method provided by the invention is simple and rapid, has high sensitivity and good accuracy and repeatability, and is suitable for preservative enterprises to be used as a basis for quality control.
Description
Technical Field
The invention belongs to the technical field of detection of caprylyl glycol, and particularly relates to a method for determining caprylyl glycol in a cosmetic preservative by using a gas chromatography.
Background
The caprylyl glycol is also called caprylyl glycol, has the main functions of an antibacterial agent and a softening agent in cosmetics and skin care products, has a risk coefficient of 1, is safe, can be used safely, has no influence on pregnant women generally, has no acne-causing property, is an 'additive-free' preservative, and is widely used in advanced mild cosmetics and skin care products.
The method for testing alcohol preservatives in cosmetics generally adopts gas chromatography and liquid chromatography, but the preservatives are added in small amount in cosmetics. For two products, namely cosmetics and preservatives, the amount of the added preservative is small generally, the detection limit in the prior art is low, and the content of the preservative, namely, the caprylyl glycol, exceeds the detection limit, so that the detection error is large. The detection limit of the existing method is low, and the content of the caprylyl glycol cannot be accurately detected. For example, in journal "Chinese test & detection" 2020.4(30-31) Chapter: the content of 1, 2-pentanediol, glyceryl monocaprylate and caprylyl glycol in the cosmetic is determined by gas chromatography, the content of three 'no-additive' preservatives is simultaneously determined by adopting the gas chromatography, the detection limit is 150mg/L, and a method for rapidly and accurately analyzing the three preservatives is established. For a compound preservative, the addition amount of the caprylyl glycol is 10-50% which is far beyond the addition amount of the cosmetic, and the error is relatively large when the method for measuring the caprylyl glycol in the cosmetic in the prior art is used for directly detecting the caprylyl glycol, so that the method for determining the preservative per se is quite essential 1 for a preservative manufacturing enterprise, and the quality control of products is more accurate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the method for determining the caprylyl glycol in the cosmetic preservative by using the gas chromatography, which has good accuracy and repetition rate and is suitable for preservative enterprises to be used as the basis for quality control.
A method for measuring caprylyl glycol in a cosmetic preservative by gas chromatography comprises the following steps:
(1) weighing the standard substance of the caprylyl glycol, placing the substance in a volumetric flask, and preparing a standard caprylyl glycol stock solution by using absolute ethyl alcohol to fix the volume;
(2) preparing the octyl glycol standard stock solution into a series of standard solutions with different concentrations of 15-300g/L by using absolute ethyl alcohol;
(3) measuring the series of standard liquids with different concentrations by adopting a capillary gas chromatography, and performing linear fitting by taking the peak area of the series of standard liquids as a horizontal coordinate x and the concentration as a vertical coordinate y to obtain a standard curve with a correlation coefficient larger than 0.999; wherein the conditions of the capillary gas chromatography are as follows: the temperature of the sample inlet is 220 ℃, and the temperature of the detector is 260 ℃; the initial temperature is 150 ℃, the temperature is kept for 1min, the temperature is raised to 240 ℃ at the speed of 20 ℃/min, and the temperature is kept for 15 min; the split ratio is 10: 1; the flow rate of combustion-supporting air is 300 mL/min; high-purity hydrogen flow of fuel gas: 30 mL/min; flow rate of carrier gas nitrogen: 1.0 mL/min; sample introduction amount: 1 mu L of the solution;
(4) weighing a preservative sample, diluting and dissolving the preservative sample by absolute ethyl alcohol to obtain a sample detection solution, detecting the sample detection solution under the condition of capillary gas chromatography, and calculating according to a peak area to obtain the content of the caprylyl glycol.
Preferably, in step (1), the concentration of the standard stock solution of the caprylyl glycol is 300 g/mL.
Preferably, in the step (2), the concentrations of the series of standard solutions with different concentrations are respectively 15g/L, 30g/L, 60g/L, 120g/L, 180g/L, 240g/L and 300 g/L.
Preferably, the concentration of the sample detection solution is 50 g/L.
Preferably, the capillary gas chromatography method adopts a chromatographic column of welch WM-Inowax, and the specification is 30m multiplied by 320 m multiplied by 0.25 m.
The purities of the air and the high-purity hydrogen are both more than 99.99 percent.
The standard substance of the caprylyl glycol is analytically pure, and the purity is 99.9%.
The invention has the advantages that:
the method provided by the invention is simple and rapid, has high sensitivity and good accuracy and repeatability, and is suitable for preservative enterprises to be used as a basis for quality control.
Drawings
FIG. 1 is a standard graph;
FIG. 2 standard solution spectra;
FIG. 3 is a sample detection profile.
Detailed Description
In the embodiment of the invention, the purities of the air and the high-purity hydrogen are both more than 99.99 percent; the caprylyl glycol standard substance is analytically pure and has a purity of 99.9%.
Example 1
A method for measuring caprylyl glycol in a cosmetic preservative by gas chromatography comprises the following steps:
(1) weighing 30g of caprylyl glycol standard substance, accurately measuring to 0.0001g, placing in a 100mL volumetric flask, and diluting to constant volume with absolute ethyl alcohol to prepare a caprylyl glycol standard stock solution with the concentration of 300 g/L;
(2) respectively transferring 0.5mL, 1mL, 2mL, 4mL, 6mL, 8mL and 10mL of the caprylyl glycol standard stock solution into a 10mL volumetric flask, using absolute ethyl alcohol to fix the volume, and respectively preparing series standard solutions of 15g/L, 30g/L, 60g/L, 120g/L, 180g/L, 240g/L and 300 g/L;
(3) measuring the series of standard solutions with different concentrations by capillary gas chromatography, taking the peak area of the series of standard solutions as abscissa x and the concentration as ordinate y, performing linear fitting to obtain standard curve of y =0.0088x +16.415 and correlation coefficient R, wherein the spectrum is shown in FIG. 22=0.9996, see fig. 1; wherein the conditions of the capillary gas chromatography are as follows: the temperature of the sample inlet is 220 ℃, and the temperature of the detector is 260 ℃; the initial temperature is 150 ℃, the temperature is kept for 1min, the temperature is raised to 240 ℃ at the speed of 20 ℃/min, and the temperature is kept for 15 min; the split ratio is 10: 1; the flow rate of combustion-supporting air is 300 mL/min; high-purity hydrogen flow of fuel gas: 30 mL/min; flow rate of carrier gas nitrogen: 1.0 mL/min; sample introduction amount: 1 mu L of the solution; the chromatographic column adopted by the capillary gas chromatography method is a welch WM-Inowax column, and the specification is 30m multiplied by 320 mu m multiplied by 0.25 mu m;
(4) weighing 0.5g of preservative sample, accurately weighing 0.0001g, placing in a 10mL volumetric flask, diluting with absolute ethyl alcohol, dissolving and fixing the volume to obtain 50g/L sample detection solution, detecting the sample detection solution under the condition of the capillary gas chromatography in the step (3), wherein the spectrum is shown in figure 3, and according to the peak area of 3887, the content of the caprylyl glycol is calculated to be 50.62 g/L.
First, repeatability detection
The detection sample adopted in the repeatability test is a preservative sample a in the prior art, and the content of the caprylyl glycol in the preservative sample a is 40 g/L;
taking 0.5g of preservative sample a, accurately obtaining 0.0001g, placing the preservative sample a in a 10mL volumetric flask, diluting and dissolving the preservative sample a with absolute ethyl alcohol to a constant volume to obtain 50g/L sample detection solution; 10 sample detection solutions are prepared in parallel for repeated tests, and are respectively numbered as sample detection solutions 1-10, the content of the caprylyl glycol is measured according to the method of the embodiment 1, and the results are shown in Table 1.
TABLE 1 repeatability test results
As can be seen from Table 1, the relative standard deviation RSD of the reproducibility was 0.26%.
Second, accuracy detection
The first 5 sample test solutions in the above-mentioned repeatability test were taken and subjected to standard addition, and the recovery rate was determined by adding 30g/L of caprylyl glycol standard substance, and the results are shown in Table 2.
TABLE 2 recovery test results
As can be seen from Table 2, the average recovery rate of the spiked sample was 100.1%, and the accuracy was high. The detection method is suitable for measuring the content of the caprylyl glycol in the cosmetic preservative.
According to the experiment, the detection limit of the method is 15g/L, and the method can be used for detecting the octyl glycol in the preservative. So as to distinguish the measurement of trace amount of caprylyl glycol in the cosmetic.
Claims (5)
1. A method for measuring the caprylyl glycol in a cosmetic preservative by gas chromatography is characterized in that: comprises the following steps:
(1) weighing the standard substance of the caprylyl glycol, placing the substance in a volumetric flask, and preparing a standard caprylyl glycol stock solution by using absolute ethyl alcohol to fix the volume;
(2) preparing the octyl glycol standard stock solution into a series of standard solutions with different concentrations of 15-300g/L by using absolute ethyl alcohol;
(3) measuring the series of standard liquids with different concentrations by adopting a capillary gas chromatography, and performing linear fitting by taking the peak area of the series of standard liquids as a horizontal coordinate x and the concentration as a vertical coordinate y to obtain a standard curve with a correlation coefficient larger than 0.999; wherein the conditions of the capillary gas chromatography are as follows: the temperature of the sample inlet is 220 ℃, and the temperature of the detector is 260 ℃; the initial temperature is 150 ℃, the temperature is kept for 1min, the temperature is raised to 240 ℃ at the speed of 20 ℃/min, and the temperature is kept for 15 min; the split ratio is 10: 1; the flow rate of combustion-supporting air is 300 mL/min; high-purity hydrogen flow of fuel gas: 30 mL/min; flow rate of carrier gas nitrogen: 1.0 mL/min; sample introduction amount: 1 mu L of the solution;
(4) weighing a preservative sample, diluting and dissolving the preservative sample by absolute ethyl alcohol to obtain a sample detection solution, detecting the sample detection solution under the condition of capillary gas chromatography, and calculating according to a peak area to obtain the content of the caprylyl glycol.
2. The method for measuring caprylyl glycol in a cosmetic preservative by gas chromatography as claimed in claim 1, wherein: in the step (1), the concentration of the standard stock solution of the caprylyl glycol is 300 g/L.
3. The method for measuring caprylyl glycol in a cosmetic preservative by gas chromatography as claimed in claim 2, wherein: in the step (2), the concentrations of the series of standard solutions with different concentrations are respectively 15g/L, 30g/L, 60g/L, 120g/L, 180g/L, 240g/L and 300 g/L.
4. The method for measuring caprylyl glycol in a cosmetic preservative by gas chromatography as claimed in claim 3, wherein: the concentration of the sample detection solution is 50 g/L.
5. The method for measuring caprylyl glycol in a cosmetic preservative by gas chromatography as claimed in claim 4, wherein: the chromatographic column adopted by the capillary gas chromatography method is a welch WM-Inowax column, and the specification is 30m multiplied by 320 mu m multiplied by 0.25 mu m.
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| CN202011528331.4A CN112526052A (en) | 2020-12-22 | 2020-12-22 | Method for measuring caprylyl glycol in cosmetic preservative by gas chromatography |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109828074A (en) * | 2019-04-15 | 2019-05-31 | 陕西省石油产品质量监督检验二站有限公司 | A kind of method of ethylene glycol content in measurement engine oil |
| 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 |
| US20200121575A1 (en) * | 2016-12-02 | 2020-04-23 | Symrise Ag | Cosmetic blends |
-
2020
- 2020-12-22 CN CN202011528331.4A patent/CN112526052A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200121575A1 (en) * | 2016-12-02 | 2020-04-23 | Symrise Ag | Cosmetic blends |
| CN109828074A (en) * | 2019-04-15 | 2019-05-31 | 陕西省石油产品质量监督检验二站有限公司 | A kind of method of ethylene glycol content in measurement engine oil |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| 唐毓萍: "气相色谱法同时测定化妆品中8种多元醇", 《香料香精化妆品》 * |
| 徐纬: "毛细管柱气相色谱法测定醇类消毒凝胶中乙醇含量", 《贵阳医学院学报》 * |
| 杜利敏等: "毛细管柱气相色谱法测定白酒中乙醇的浓度", 《医药论坛杂质》 * |
| 陈苏敏等: "气相色谱法测定化妆品中1,2-戊二醇、单辛酸甘油酯、辛甘醇的含量", 《中国检验检测》 * |
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