Method for simultaneous detection of multiple polyols in cosmetic products

CN120028463BActive Publication Date: 2026-10-09SHANGHAI INST FOR FOOD & DRUG CONTROL
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202510315440.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-03-17
Publication Date
2026-10-09
Estimated Expiration
2045-03-17

AI Technical Summary

Technical Problem

文献多采用气相色谱法测定多元醇,但由于气相色谱仅通过保留时间定性,容易造成结果假阳性

Benefits of technology

[0045] The method of this invention can be used to simultaneously analyze the content of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butylene glycol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in cosmetics. This detection method is simple to operate, rapid in analysis, highly specific, and has high separation. It can be used as a detection method for polyol moisturizers in cosmetics, providing technical support for the analysis of moisturizing functional raw materials in cosmetics.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN120028463B_ABST
    Figure CN120028463B_ABST
Patent Text Reader

Abstract

The application discloses a method for simultaneously detecting multiple polyols in cosmetics. The method is used for simultaneously analyzing the contents of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propylene glycol, 1,2-pentanediol, dipropylene glycol, glycerol and 1,2-hexanediol in cosmetics, and has the advantages of simple operation, rapid analysis, strong specificity, high separation degree and the like. The detection method can be used as a detection method for polyol moisturizers in cosmetics, and provides technical support for analyzing moisturizing functional raw materials of cosmetics.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This application relates to the field of analytical testing, and in particular to a method for the simultaneous detection of multiple polyols in cosmetics. Background Technology

[0002] Moisturizing has always been one of the basic requirements of skincare products. Even with a plethora of new skincare products emerging today, moisturizing remains the most sought-after feature by consumers. [1] The stratum corneum of the skin needs 10% to 30% moisture to maintain smoothness and prevent cracking. With the implementation of a series of regulations in recent years, such as the "Cosmetics Supervision and Management Regulations" and the "Cosmetics Efficacy Claim Evaluation Standards," product efficacy claims are becoming increasingly standardized and scientific, and moisturizing claims require data support.

[0003] Polyol moisturizers are an important class of moisturizing ingredients in cosmetics, increasing the content of secondary bound water in the stratum corneum. Polyol molecules contain two or more hydroxyl groups (-OH), which form hydrogen bonds with water molecules, absorbing and locking in moisture, reducing water evaporation from the skin surface, and simultaneously forming a hydrating film on the skin surface to maintain skin hydration and softness, thus achieving a hygroscopic and moisturizing effect. Commonly used polyol moisturizers include glycerin, propylene glycol, butylene glycol, and 1,2-hexanediol, all of which are listed as cosmetic ingredients in my country's "Catalogue of Used Cosmetic Ingredients (2021 Edition)" and also in the "Chinese Catalogue of International Cosmetic Ingredient Standards."

[0004] Excessive use of polyol moisturizers carries certain risks. High concentrations of propylene glycol-based substances can cause burning, stinging, or itching, leading to skin irritation. Furthermore, due to their high lipid solubility and penetrability, long-term use can damage the epidermis and sebum structure. Accumulation of polyols in the body can cause damage to the lungs, heart, and central nervous system, potentially leading to vomiting, convulsions, neurological disorders, and birth defects. Chinese regulations have not yet established management limits for polyol moisturizers in cosmetics. The "Cosmetic Safety Technical Specifications," national standards, and supplementary testing methods do not include methods for detecting polyols in cosmetics. While literature often uses gas chromatography to determine polyols, this method relies solely on retention time for qualitative analysis, which can easily result in false positives. Summary of the Invention

[0005] The purpose of this application is to provide a method for simultaneously detecting multiple polyols in cosmetics.

[0006] To address the aforementioned technical problems, a first aspect of this application provides a method for simultaneously detecting multiple polyols in cosmetics. The method includes the steps of: simultaneously detecting the contents of 1,2-propanediol, 1,3-propanediol, butylene glycol, and methylpropanediol in the cosmetic to be tested using gas chromatography-mass spectrometry (GC-MS), wherein the mass spectrometry conditions of the GC-MS include:

[0007] 45 m / z, 61 m / z, and 29 m / z were selected as characteristic ions of 1,2-propanediol.

[0008] 57 m / z, 28 m / z and 31 m / z were selected as characteristic ions of 1,3-propanediol;

[0009] 43 m / z, 72 m / z, and 57 m / z were selected as characteristic ions of butanediol.

[0010] 42 m / z, 57 m / z, and 31 m / z were selected as characteristic ions of methylpropanediol.

[0011] In some preferred embodiments, the method simultaneously detects the contents of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butanediol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol.

[0012] In some preferred embodiments, the mass spectrometry conditions of the gas chromatography-mass spectrometry system include: selecting 31 m / z as the qualitative ion of ethylene glycol, and selecting 43 m / z and 62 m / z as the quantitative ions of ethylene glycol;

[0013] 45 m / z was selected as the qualitative ion of 1,2-propanediol, and 61 m / z and 29 m / z were selected as quantitative ions.

[0014] 57 m / z was selected as the qualitative ion of 1,3-propanediol, and 28 m / z and 31 m / z were selected as the quantitative ions of 1,3-propanediol.

[0015] 43 m / z was selected as the qualitative ion of butanediol, and 72 m / z and 57 m / z were selected as the quantitative ions of butanediol.

[0016] 42* was selected as the qualitative ion for methylpropanediol, and 57 m / z and 31 m / z were selected as the quantitative ions for methylpropanediol.

[0017] 55 m / z was selected as the qualitative ion of 1,2-pentanediol, and 73 m / z and 43 m / z were selected as the quantitative ions of 1,2-pentanediol.

[0018] 45 m / z was selected as the qualitative ion for dipropylene glycol, and 89 m / z and 59 m / z were selected as the quantitative ions for dipropylene glycol.

[0019] Select 61 m / z as the qualitative ion for glycerol, and select 43 m / z and 31 m / z as the quantitative ions for glycerol; and / or

[0020] 69 m / z was selected as the qualitative ion for 1,2-hexanediol, and 87 m / z and 41 m / z were selected as the quantitative ions for 1,2-hexanediol.

[0021] In some preferred embodiments, the mass spectrometry conditions of the gas chromatography-mass spectrometry system include: ionization mode: EI; ion source temperature: 230°C; mass spectrometry interface: 240°C; solvent delay: 5 min; detector voltage: tuning voltage; detection mode: selected ion monitoring (SIM).

[0022] In some preferred embodiments, the chromatographic conditions of the gas chromatography-mass spectrometry system include: selecting a medium polarity column as the analytical column.

[0023] In some preferred embodiments, the chromatographic conditions of the gas chromatography-mass spectrometry system include: selecting a DB-624 column as the analytical column.

[0024] In some preferred embodiments, the chromatographic conditions of the gas chromatography-mass spectrometry system include: setting a programmed temperature increase, with an initial temperature of approximately 50°C, then increasing the temperature at 10°C / min to 140°C and holding for at least 1 min, increasing the temperature at 8°C / min to 185°C and holding for at least 5 min, and increasing the temperature at 20°C / min to 230°C and holding for at least 1.13 min.

[0025] In some preferred embodiments, the chromatographic conditions of the gas chromatography-mass spectrometry (GC-MS) system include:

[0026] Inlet temperature: 230℃

[0027] Column flow rate: 1.0 mL / min

[0028] Sample introduction method: split injection;

[0029] Split ratio: (10-30):1, (e.g., 20:1).

[0030] In some preferred embodiments, the method further includes the step of selecting a suitable pretreatment method based on the matrix type of the cosmetic product to be tested.

[0031] In some preferred embodiments, when the cosmetic to be tested is a liquid water-based product, a cream, lotion, or powder, the pretreatment method includes the steps of dissolving the sample in methanol and then taking the supernatant for testing.

[0032] In some preferred embodiments, when the cosmetic to be tested is a liquid water-based product, cream, lotion, or powder, the pretreatment method includes the following steps: accurately weigh 0.25 g of the sample (accurate to 0.0001 g), place it in a 25 mL plastic centrifuge tube, add methanol to disperse the sample, vortex for 30 seconds and mix thoroughly, sonicate for 10 minutes, cool to room temperature, add methanol to make up to the mark, vortex to mix, centrifuge at 10000 r / min for 5 minutes, take an appropriate amount of the supernatant, filter it through a 0.22 μm organic filter membrane, and keep the filtrate for later use.

[0033] In some preferred embodiments, when the cosmetic to be tested is a liquid oil-based product, the pretreatment method includes the steps of taking the sample to be tested, adding hexane, then adding methanol to dissolve it, and then taking the supernatant for testing.

[0034] In some preferred embodiments, when the cosmetic to be tested is a liquid oil-based product, the pretreatment method includes the following steps: accurately weigh 0.25 g of the sample (accurate to 0.0001 g), place it in a 25 mL plastic centrifuge tube, add 2 mL of n-hexane, disperse it on a vortex mixer, then add 3 mL of methanol, vortex for 1 min, centrifuge at 4000 r / min for 5 min, aspirate the lower layer solution into a 25 mL stoppered colorimetric tube, extract the upper layer once again with 3 mL of methanol, combine the two solutions, add methanol to make up to the mark, vortex to mix, centrifuge at 10000 r / min for 5 min, take an appropriate amount of supernatant, filter it through a 0.22 μm organic filter membrane, and keep the filtrate for later use.

[0035] In some preferred embodiments, when the cosmetic to be tested is a wax-based product, the pretreatment method includes the steps of taking the sample to be tested, adding tetrahydrofuran, then adding methanol to dissolve it, and then taking the supernatant for detection.

[0036] In some preferred embodiments, when the cosmetic to be tested is a wax-based product, the pretreatment method includes the following steps: accurately weigh 0.25 g of the sample (accurate to 0.0001 g), place it in a 25 mL plastic centrifuge tube, add 2 mL of tetrahydrofuran to disperse the sample, add an appropriate amount of methanol, vortex for 30 s and mix thoroughly, sonicate for 10 min, cool to room temperature, add methanol to make up to the mark, vortex to mix, centrifuge at 10000 r / min for 5 min, take an appropriate amount of supernatant, filter through a 0.22 μm organic filter membrane, and keep the filtrate for later use.

[0037] In some preferred embodiments, the method simultaneously detects ethylene glycol, 1,2-propanediol, 1,3-propanediol, butanediol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol, with recoveries ranging from 95.0% to 105.6%.

[0038] In some preferred embodiments, after selecting a suitable pretreatment method based on the matrix type of the cosmetic to be tested, the method further includes the following steps:

[0039] Detect standard solutions of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butanediol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol and plot standard curves;

[0040] The cosmetic product to be tested was analyzed, and the contents of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butylene glycol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in the cosmetic product were obtained according to the standard curve.

[0041] In some preferred embodiments, the cosmetic to be tested is selected from at least one of liquid water-based, cream / lotion, liquid oil-based, wax-based, and powder-based products.

[0042] In some preferred embodiments, the cosmetic to be tested is any cosmetic that is labeled or advertised as moisturizing.

[0043] In some preferred embodiments, the cosmetic is selected from at least one of toner, body lotion, serum, face cream, loose powder, essential oil, face mask, hand mask, eye patch, spray, lipstick, lip mask, sunscreen, makeup primer, foundation, facial cleanser, hand cream, shampoo, conditioner, hair oil, shower gel, nail polish, and body oil.

[0044] Based on the prior art, the present invention has at least the following advantages:

[0045] The method of this invention can be used to simultaneously analyze the content of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butylene glycol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in cosmetics. This detection method is simple to operate, rapid in analysis, highly specific, and has high separation. It can be used as a detection method for polyol moisturizers in cosmetics, providing technical support for the analysis of moisturizing functional raw materials in cosmetics.

[0046] It should be understood that, within the scope of this application, the above-described technical features of this application and the technical features specifically described below (such as in the embodiments) can be combined with each other to form new or preferred technical solutions. Due to space limitations, they will not be described in detail here. Attached Figure Description

[0047] One or more embodiments are illustrated by way of example with reference to the accompanying drawings, and these illustrative descriptions do not constitute a limitation on the embodiments.

[0048] Figure 1 This is the gas chromatography-mass spectrum of ethylene glycol;

[0049] Figure 2 This is a gas chromatography-mass spectrum of 1,2-propanediol;

[0050] Figure 3 This is a gas chromatography-mass spectrum of 1,3-propanediol;

[0051] Figure 4 This is the gas chromatography-mass spectrum of butanediol;

[0052] Figure 5 This is the gas chromatography-mass spectrum of methylpropanediol;

[0053] Figure 6 This is the gas chromatography-mass spectrum of 1,2-pentanediol;

[0054] Figure 7 This is the gas chromatography-mass spectrum of dipropylene glycol;

[0055] Figure 8 This is the gas chromatography-mass spectrum of glycerol;

[0056] Figure 9 This is a gas chromatography-mass spectrum of 1,2-hexanediol. Detailed Implementation

[0057] Through extensive and in-depth research, the inventors have optimized chromatographic analysis by screening characteristic ion pairs to effectively separate multiple isomers in cosmetics. This method can be used to simultaneously analyze the content of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butylene glycol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in cosmetics. This detection method is simple to operate, rapid, highly specific, and has high separation. It can be used as a detection method for polyol moisturizers in cosmetics, providing technical support for the analysis of moisturizing ingredients in cosmetics.

[0058] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the present application is further described below in conjunction with specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of this application. Experimental methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions or as recommended by the manufacturer. Unless otherwise stated, percentages and parts are weight percentages and weight parts. Unless otherwise specified, the experimental materials and reagents used in the following embodiments are commercially available.

[0059] Unless otherwise specified, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains. It should be noted that the terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the exemplary embodiments of this application.

[0060] Example 1

[0061] 1. Instruments, reagents and materials

[0062] Ethylene glycol standard (99.5% purity) was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; 1,2-propanediol standard (99.5% purity) was purchased from Shanghai Anpu Laboratory Technology Co., Ltd.; 1,3-propanediol standard (99.5% purity) was purchased from Shanghai Anpu Laboratory Technology Co., Ltd.; butylene glycol standard (99.0% purity) was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; methylpropanediol standard (98.0% purity) was purchased from Shanghai Maclean's Biochemical Technology Co., Ltd.; 1,2-pentanediol standard (98.0% purity) was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; dipropylene glycol standard (95.0% purity) was purchased from Shanghai Maclean's Biochemical Technology Co., Ltd.; glycerol standard (99.7% purity) was purchased from Shanghai Maclean's Biochemical Technology Co., Ltd.; 1,2-hexanediol standard (96.0% purity) was purchased from Shanghai Anpu Laboratory Technology Co., Ltd. Methanol was purchased from Thermo Fisher Scientific, chromatographic grade; n-hexane was purchased from Thermo Fisher Scientific, chromatographic grade; acetone was purchased from Thermo Fisher Scientific, chromatographic grade; water was ultrapure water. The equipment included a Shimadzu GC-2010plus gas chromatograph, a Shimadzu GCMS-TQ8040 mass spectrometer, an IKAVORTEX4 vortex mixer, an Eppendorf 5810R centrifuge, a Mettler Toledo electronic balance, and an Emerson ultrasonic transducer. A 0.22 μm microporous filter membrane (Nylon 6, Navigator) was used.

[0063] 2. Testing Process

[0064] Preparation of standards: Accurately weigh 100 mg each of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butanediol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol standards, place them in the same 10 mL volumetric flask, dissolve them in methanol, and dilute to the mark. Shake well to prepare the stock solutions of the nine polyol standards.

[0065] Preparation of standard solutions: Accurately pipette an appropriate amount of the standard stock solution and dilute it with methanol to prepare a series of standard working solutions containing methylpropanediol at concentrations of 20 μg / mL, 50 μg / mL, 100 μg / mL, 200 μg / mL, 400 μg / mL, and 600 μg / mL.

[0066] Sample pretreatment:

[0067] For liquid water-based, cream / lotion, and powder samples: accurately weigh 0.25 g of the sample (accurate to 0.0001 g), place it in a 25 mL plastic centrifuge tube, add methanol to disperse the sample, vortex for 30 s and mix thoroughly, sonicate for 10 min, cool to room temperature, add methanol to make up to the mark, vortex to mix, centrifuge at 10000 r / min for 5 min, take an appropriate amount of supernatant, filter through a 0.22 μm organic filter membrane, and keep the filtrate for later use.

[0068] For liquid oil-based samples: Accurately weigh 0.25 g of the sample (accurate to 0.0001 g), place it in a 25 mL plastic centrifuge tube, add 2 mL of n-hexane, disperse it on a vortex mixer, then add 3 mL of methanol, vortex for 1 min, centrifuge at 4000 r / min for 5 min, and transfer the lower layer solution to a 25 mL stoppered colorimetric tube. Extract the upper layer once more with 3 mL of methanol, combine the two solutions, add methanol to the mark, vortex to mix, centrifuge at 10000 r / min for 5 min, take an appropriate amount of the supernatant, filter it through a 0.22 μm organic filter membrane, and keep the filtrate for later use.

[0069] For wax-based samples: Accurately weigh 0.25 g of the sample (accurate to 0.0001 g), place it in a 25 mL plastic centrifuge tube, add 2 mL of tetrahydrofuran to disperse the sample, add an appropriate amount of methanol, vortex for 30 s and mix thoroughly, sonicate for 10 min, cool to room temperature, add methanol to the mark, vortex to mix, centrifuge at 10000 r / min for 5 min, take an appropriate amount of supernatant, filter through a 0.22 μm organic filter membrane, and keep the filtrate for later use.

[0070] Detection: The series of standard solutions in (2) and the filtrate in (3) were injected into a gas chromatograph for quantitative analysis.

[0071] 1) Gas chromatographic parameters

[0072] Chromatographic column: DB-624 gas chromatographic column (30m×0.25mm×1.4μm); injection port temperature: 230℃; column flow rate: 1.0mL / min; injection mode: split injection; split ratio: 20:1; injection volume: 1μL; carrier gas: high-purity helium (99.999%).

[0073] The temperature program is as follows: Initial temperature 50℃, hold for 2 min, increase to 140℃ at 10℃ / min, hold for 1 min, increase to 185℃ at 8℃ / min, hold for 5 min, increase to 230℃ at 20℃ / min, and hold for 1.13 min.

[0074] 2) Mass spectrometry parameters

[0075] Ionization mode: EI; Ion source temperature: 230℃; Mass spectrometry interface: 240℃; Solvent delay: 5 min; Detector voltage: Tuned voltage; Detection mode: Selected ion monitoring (SIM); Compound information is detailed in Table 3. Ions with high response and few interferences were used as quantitative ions, and the rest were used as qualitative ions.

[0076] Table 3. GC-MS parameters of nine polyols including methylpropanediol.

[0077]

[0078] Note: * indicates quantitative ions.

[0079] The linear equation, correlation coefficient, linear range, and detection limit of methylpropanediol are shown in Table 4.

[0080] Table 4. Linear equations, correlation coefficients, linear ranges, and detection limits for nine polyols, including methylpropanediol.

[0081]

[0082] See test results Figure 1-9 .

[0083] 3. Optimization of test conditions

[0084] 3.1 Selection of chromatographic column and optimization of temperature program

[0085] During the analysis, due to the similarity of compound structures, similar retention times, and low molecular weight, identical fragments are easily generated. To ensure accurate qualitative and quantitative analysis of the compounds, it is necessary to ensure effective separation of each component on the chromatographic column. Separation performance tests were conducted using DB-624 column (30m × 0.25mm × 1.4μm), DB-5MS column (30m × 0.25mm × 0.25μm), and INNOWAX column (30m × 0.25mm × 0.25μm), respectively.

[0086] The results showed that the DB-5MS column, being a non-polar column, is unsuitable for analyzing highly polar compounds such as propylene glycol and glycerol, resulting in peak tailing. While the highly polar INNOWAX column yielded good peak shapes, complete separation of 1,2-pentanediol and 1,3-propanediol was not achieved. Selecting the DB-624 column, suitable for volatile compounds, resulted in good peak shapes. Adjusting the temperature program, lowering the initial temperature to 50℃, and slowly increasing the temperature allowed for good separation and peak shapes for all nine compounds.

[0087] 3.2 Selection of ion pairs

[0088] Since the molecular weights of the nine compounds are concentrated between 62 and 135, and there are two pairs of isomers: 1,2-propanediol and 1,3-propanediol, and butanediol and methylpropanediol, in addition to ensuring effective separation of chromatographic peaks, it is necessary to make every effort to select different characteristic ions to ensure the accuracy of qualitative and quantitative analysis. The characteristic ions for 1,2-propanediol and 1,3-propanediol are 45, 61, 29 and 57, 28, 31, respectively; the characteristic ions for butanediol and methylpropanediol are 43, 72, 57 and 42, 57, 31, respectively.

[0089] 3.3 Solvent Selection

[0090] Methanol, acetonitrile, and acetone were used as solvents, and all yielded good chromatographic peaks on a DB-624 column, with no significant differences in the responses of the nine components. The three solvents were also investigated as extraction and dispersion solvents for the samples, and the recoveries of all three met the requirements. Considering the toxicity of acetonitrile and acetone, methanol was ultimately chosen as both the standard solvent and the sample extraction solvent.

[0091] 4. Precision and stability studies

[0092] The instrument precision was assessed by injecting mixed standard solutions at concentrations of 100 μg / mL, 200 μg / mL, and 400 μg / mL six times consecutively. The results showed that the peak area RSD was less than 5%, indicating good instrument precision. Peak area RSD was also measured on days 1, 2, 3, 4, and 5 using mixed standard solutions at concentrations of 100 μg / mL, 200 μg / mL, and 400 μg / mL, as well as a blank matrix spiking solution. The peak area RSD was less than 5%, indicating that the nine polyols remained stable over five days.

[0093] Example 2

[0094] Five commercially available cosmetic bases were used as test subjects, spiked at concentrations of 10 mg / g, 20 mg / g, and 40 mg / g, respectively. Parallel experiments (n=6) were conducted, and the recoveries and relative deviations (RSD%) were determined. The results are shown in Table 5. The results indicate that the recoveries of the nine components ranged from 95.68% to 105.57% under high, medium, and low spiked concentrations, with RSDs (n=6) ranging from 1.40% to 7.25%. This demonstrates that the recovery results of this method are good.

[0095] Table 5 Recovery rate results (n=6)

[0096]

[0097]

[0098] Example 3

[0099] Using this testing method, 20 batches of commercially available products containing polyol moisturizers on their labels were selected, covering liquid oil-based, cream, lotion, wax-based, powder, and liquid water-based moisturizing cosmetics (toner, serum, face cream, loose powder, facial oil, etc.). Among them, 11 batches were found to contain polyol moisturizers. The test results are detailed in the table below.

[0100] Table 6. Results of Positive Samples

[0101]

[0102] The foregoing description illustrates and illustrates the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments, which are merely preferred embodiments and should not be construed as limiting the scope of the invention. All equivalent changes and modifications made in accordance with the scope of the patent and the description should still fall within the scope of the present invention. The scope of protection of this invention is defined by the appended claims and their equivalents.

[0103] Those skilled in the art will understand that the above-described embodiments are specific implementations of this application, and in practical applications, various changes can be made in form and detail without departing from the spirit and scope of this application.

Claims

1. A method for simultaneously detecting multiple polyols in cosmetics, characterized in that, The method includes the steps of: simultaneously detecting the contents of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butylene glycol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in the cosmetic sample using gas chromatography-mass spectrometry (GC-MS), wherein the mass spectrometry conditions of the GC-MS include: 31 m / z was selected as the qualitative ion of ethylene glycol, and 43 m / z and 62 m / z were selected as the quantitative ions of ethylene glycol. 45 m / z was selected as the qualitative ion of 1,2-propanediol, and 61 m / z and 29 m / z were selected as quantitative ions. 57 m / z was selected as the qualitative ion for 1,3-propanediol, and 28 m / z and 31 m / z were selected as the quantitative ions for 1,3-propanediol. 43 m / z was selected as the qualitative ion of butanediol, and 72 m / z and 57 m / z were selected as the quantitative ions of butanediol. 42 m / z was selected as the qualitative ion for methylpropanediol, and 57 m / z and 31 m / z were selected as the quantitative ions for methylpropanediol. 55 m / z was selected as the qualitative ion for 1,2-pentanediol, and 73 m / z and 43 m / z were selected as the quantitative ions for 1,2-pentanediol. 45 m / z was selected as the qualitative ion for dipropylene glycol, and 89 m / z and 59 m / z were selected as the quantitative ions for dipropylene glycol. 61 m / z was selected as the qualitative ion for glycerol, and 43 m / z and 31 m / z were selected as the quantitative ions for glycerol; and 69 m / z was selected as the qualitative ion for 1,2-hexanediol, and 87 m / z and 41 m / z were selected as the quantitative ions for 1,2-hexanediol. The chromatographic conditions of the gas chromatography-mass spectrometry system include: selecting a medium polarity column as the analytical column; The chromatographic conditions of the gas chromatography-mass spectrometry system include: setting a programmed temperature increase, with an initial temperature of approximately 50°C, then increasing the temperature at 10°C / min to 140°C and holding for at least 1 min, increasing the temperature at 8°C / min to 185°C and holding for at least 5 min, and increasing the temperature at 20°C / min to 230°C and holding for at least 1.13 min. The method also includes the step of selecting a suitable pretreatment method based on the matrix type of the cosmetic to be tested; When the cosmetic to be tested is a liquid water-based product, cream, lotion, or powder, the pretreatment method includes the steps of dissolving the sample in methanol and then taking the supernatant for testing. When the cosmetic to be tested is a liquid oil-based product, the pretreatment method includes the steps of taking the sample to be tested, adding hexane, then adding methanol to dissolve it, and then taking the supernatant for testing. When the cosmetic to be tested is a wax-based product, the pretreatment method includes the steps of taking the sample to be tested, adding tetrahydrofuran, then adding methanol to dissolve it, and then taking the supernatant for testing.

2. The method according to claim 1, characterized in that, The medium polarity chromatographic column is a DB-624 column.

3. The method according to claim 1, characterized in that, The cosmetic product to be tested is selected from at least one of the following: liquid water-based, cream / lotion, liquid oil-based, wax-based, and powder.

4. The method according to claim 1, characterized in that, After selecting a suitable pretreatment method based on the matrix type of the cosmetic to be tested, the method also includes the following steps: Detect standard solutions of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butanediol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol and plot standard curves; The cosmetic product to be tested was analyzed, and the contents of ethylene glycol, 1,2-propanediol, 1,3-propanediol, butylene glycol, methylpropanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in the cosmetic product were obtained according to the standard curve.

5. The method according to claim 1, characterized in that, The cosmetics are selected from at least one of the following: toner, body lotion, serum, face cream, loose powder, essential oil, face mask, hand mask, eye patch, spray, lipstick, lip mask, sunscreen, makeup primer, foundation, facial cleanser, hand cream, shampoo, conditioner, hair oil, shower gel, nail polish, and body oil.

Citation Information

Patent Citations

  • Method for simultaneous determination of eight glycol ether compounds in cosmetics

    CN108037231A

  • Researching method for determining components of grease in cosmetics

    CN112684046A