Method for simultaneously detecting multiple polyols in cosmetics
By using gas chromatography mass spectrometer (GC-MS) to detect the content of various polyols in cosmetics, the problems of false positive detection and lack of scientific methods in the prior art are solved, and the effects of high accuracy and rapid analysis are achieved.
Patent Information
- Application Number
- CN202510315440.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-17
- Publication Date
- 2025-05-23
AI Technical Summary
The prior art is difficult to effectively detect the content of various polyols in cosmetics, especially since gas chromatography can easily lead to false positive results, and there is a lack of scientific detection methods and management limits.
The gas chromatography mass spectrometry combined instrument (GC-MS) was used to simultaneously detect the content of polyols such as 1,2-propanediol, 1,3-propanediol, butanediol, methylpropanediol and other polyols in cosmetics. By selecting characteristic ions and optimizing chromatographic conditions, the accuracy and resolution of the detection were improved.
It realizes the simultaneous detection of a variety of polyols in cosmetics, with simple operation and fast analysis, high specificity and resolution, and can effectively support the detection and analysis of polyol moisturizers in cosmetics.
Smart Images

Figure CN120028463A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the field of analysis and detection, and in particular to a method for simultaneously detecting multiple polyols in cosmetics. Background Art
[0002] Moisturizing has always been one of the basic requirements of skin care products. Today, with many new functions emerging like mushrooms after rain, moisturizing is still the function that consumers pay the most attention to. [1] The stratum corneum of the skin needs 10% to 30% of water to keep the skin smooth and chapped. With the implementation of a series of laws and regulations in recent years, such as the "Regulations on the Supervision and Administration of Cosmetics" and the "Standards for the Evaluation of Cosmetic Efficacy Claims", the efficacy claims of products have become more standardized and scientific, and the moisturizing claims of products need data support.
[0003] Polyol moisturizers are an important type of moisturizing ingredient in cosmetics, which can increase 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 through hydroxyl groups, absorb and lock in moisture, reduce the evaporation of moisture on the skin surface, and form a hydration film on the skin surface to maintain the moisture and softness of the skin, thereby achieving hygroscopic and moisturizing effects. Commonly used polyol moisturizers include glycerin, propylene glycol, butylene glycol, 1,2-hexanediol, etc., which are all included as cosmetic raw materials in my country's "Catalogue of Used Cosmetic Raw Materials (2021 Edition)", and are also included in the "Chinese Catalogue of International Cosmetic Raw Materials Standards".
[0004] There are certain risks in overusing polyol moisturizers. When propylene glycol is added at too high a concentration, it will produce a burning, stinging or itching sensation, causing skin irritation. At the same time, due to the strong fat solubility and permeability of polyols, long-term use can also damage the epidermis and sebum structure. As polyols accumulate in the body, they can cause damage to the lungs, heart and central nervous system, and in severe cases cause vomiting, convulsions, neurosis, embryonic malformations and other diseases. my country's laws and regulations have not yet established management limits for polyol moisturizers in cosmetics. The "Technical Specifications for Safety of Cosmetics", national standards, supplementary inspection methods and other statutory standards do not include the detection methods of polyols in cosmetics. Most literature uses gas chromatography to determine polyols, but since gas chromatography is only qualitative by retention time, it is easy to cause false positive results. Summary of the invention
[0005] The purpose of this application is to provide a method for simultaneously detecting multiple polyols in cosmetics.
[0006] In order to solve the above technical problems, the first aspect of the present application provides a method for simultaneously detecting multiple polyols in cosmetics, the method comprising the steps of: using a gas chromatograph-mass spectrometer to simultaneously detect the contents of 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, and methylpropanediol in the cosmetics to be tested, and the mass spectrometry conditions of the gas chromatograph-mass spectrometer include:
[0007] 45 m / z , 61 m / z , and 29 m / z were selected as characteristic ions of 1,2-propylene glycol;
[0008] 57 m / z , 28 m / z , and 31 m / z were selected as characteristic ions of 1,3-propanediol;
[0009] 43m / z, 72m / z, and 57m / 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-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol.
[0012] In some preferred embodiments, the mass spectrometry conditions of the gas chromatography-mass spectrometer include: selecting 31m / z as the qualitative ion of ethylene glycol, and selecting 43m / z and 62m / z as the quantitative ions of ethylene glycol;
[0013] Select 45*m / z as the qualitative ion of 1,2-propylene glycol, and select 61m / z and 29m / z as the quantitative ions;
[0014] Select 57*m / z as the qualifier ion of 1,3-propylene glycol, and 28m / z and 31m / z as the quantitative ions of 1,3-propylene glycol;
[0015] Select 43*m / z as the qualitative ion of butanediol, and select 72m / z and 57m / z as the quantitative ions of butanediol;
[0016] Select 42* as the methylpropanediol qualitative ion, and select 57m / z and 31m / z as the methylpropanediol quantitative ions;
[0017] Select 55*m / z as the qualifier ion for 1,2-pentanediol, and select 73m / z and 43m / z as the quantitative ions for 1,2-pentanediol;
[0018] Select 45*m / z as the DPG qualitative ion, and select 89m / z and 59m / z as the DPG quantitative ions;
[0019] Select 61*m / z as the glycerol qualitative ion, and select 43m / z and 31m / z as the glycerol quantitative ions; and / or
[0020] 69*m / z was selected as the qualifier ion for 1,2-hexanediol, and 87m / z and 41m / z were selected as the quantitative ions for 1,2-hexanediol.
[0021] In some preferred embodiments, the mass spectrometry conditions of the gas chromatograph-mass spectrometer include: ionization 230 mode: EI; ion source temperature: 230°C, mass spectrometry interface: 240°C, solvent delay: 5min, detector voltage: tuning voltage, detection mode: selected ion monitoring (SIM).
[0022] In some preferred embodiments, the chromatographic conditions of the gas chromatography-mass spectrometry include: selecting a medium polarity chromatographic column as the analytical column.
[0023] In some preferred embodiments, the chromatographic conditions of the gas chromatograph-mass spectrometer include: selecting a DB-624 chromatographic column as an analytical column.
[0024] In some preferred embodiments, the chromatographic conditions of the gas chromatograph-mass spectrometer include: setting a temperature program with an initial temperature of approximately 50°C, then heating to 140°C at 10°C / min and holding for at least 1 min, heating to 185°C at 8°C / min and holding for at least 5 min, and heating to 230°C at 20°C / min and holding for at least 1.13 min.
[0025] In some preferred embodiments, the chromatographic conditions of the gas chromatography-mass spectrometry instrument include:
[0026] Inlet temperature: 230°C,
[0027] Column flow rate: 1.0mL / min,
[0028] Injection method: split injection;
[0029] Split ratio: (10-30):1, (e.g. 20:1).
[0030] In some preferred embodiments, the method further comprises the step of selecting a suitable pre-treatment method according to the matrix type of the cosmetic to be tested.
[0031] In some preferred embodiments, when the cosmetic to be tested is a liquid water-based type, a cream lotion type or a powder type, the pretreatment method includes the steps of taking the sample to be tested, adding methanol to dissolve it, and then taking the supernatant for testing.
[0032] In some preferred schemes, when the cosmetic to be tested is a liquid water-based type, a cream emulsion type or a powder type, the pretreatment method comprises the steps of accurately weighing 0.25 g of the sample (accurate to 0.0001 g), placing it in a 25 mL plastic centrifuge tube, adding methanol to disperse the sample, vortexing for 30 seconds and fully mixing, ultrasonicating for 10 minutes, cooling to room temperature and adding methanol to the scale, vortexing and mixing, centrifuging at 10000 r / min for 5 minutes, taking an appropriate amount of supernatant, passing it through a 0.22 μm organic filter membrane, and setting the filtrate aside.
[0033] In some preferred embodiments, when the cosmetic to be tested is a liquid oil-based cosmetic, the pretreatment method includes the steps of first adding n-hexane to the sample to be tested and then adding methanol to dissolve it, and then taking the supernatant for testing.
[0034] In some preferred schemes, when the cosmetic to be tested is a liquid oil-based type, the pretreatment method includes the steps of: accurately weighing 0.25g of the sample (accurate to 0.0001g), placing it in a 25mL plastic centrifuge tube, adding 2mL of n-hexane, dispersing it on a vortexer, then adding 3mL of methanol, vortexing for 1min, centrifuging at 4000r / min for 5min, aspirating the lower layer solution into a 25mL stoppered colorimetric tube, repeatedly extracting the upper layer with 3mL of methanol once, combining the two solutions, adding methanol to the scale, vortexing to mix, centrifuging at 10000r / min for 5min, taking an appropriate amount of supernatant, passing it through a 0.22μm organic filter membrane, and setting the filtrate aside.
[0035] In some preferred embodiments, when the cosmetics to be tested are wax-based, the pretreatment method includes the steps of first adding tetrahydrofuran to the sample to be tested and then adding methanol to dissolve it, and then taking the supernatant for testing.
[0036] In some preferred schemes, when the cosmetic to be tested is wax-based, the pretreatment method includes the steps of accurately weighing 0.25 g of the sample (accurate to 0.0001 g), placing it in a 25 mL plastic centrifuge tube, adding 2 mL of tetrahydrofuran to disperse the sample, adding an appropriate amount of methanol, vortexing for 30 seconds and fully mixing, ultrasonicating for 10 minutes, cooling to room temperature and adding methanol to the scale, vortexing and mixing, centrifuging at 10000 r / min for 5 minutes, taking an appropriate amount of supernatant, passing it through a 0.22 μm organic filter membrane, and setting the filtrate aside.
[0037] In some preferred embodiments, the method simultaneously detects ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol, and the recovery rates are all in the range of 95.0% to 105.6%.
[0038] In some preferred embodiments, after selecting a suitable pre-treatment method according to the matrix type of the cosmetic to be tested, the method further comprises the following steps:
[0039] Detect ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol and 1,2-hexanediol standard solutions and draw standard curves;
[0040] The cosmetics to be tested are detected, and the contents of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol and 1,2-hexanediol in the cosmetics to be tested are 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 emulsion, liquid oil-based, wax-based, and powder.
[0042] In some preferred embodiments, the cosmetic to be tested is any cosmetic with moisturizing properties in its label or advertisement.
[0043] In some preferred embodiments, the cosmetics are selected from at least one of toner, body lotion, essence, face cream, loose powder, essential oil, facial mask, hand mask, eye patch, spray, lipstick, lip mask, sunscreen, primer, liquid foundation, facial cleanser, hand cream, shampoo, conditioner, hair essential 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 the present invention can be used to simultaneously analyze the contents of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in cosmetics. The detection method is simple to operate, fast to analyze, highly specific, and has a high degree of separation. It can be used as a detection method for polyol moisturizers in cosmetics, and provides 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-mentioned technical features of this application and the technical features specifically described below (such as embodiments) can be combined with each other to form a new or preferred technical solution. Due to space limitations, they will not be described one by one here. BRIEF DESCRIPTION OF THE DRAWINGS
[0047] One or more embodiments are exemplarily described by the pictures in the corresponding drawings, and these exemplary descriptions do not constitute limitations on the embodiments.
[0048] Figure 1 is the gas chromatography-mass spectrum of ethylene glycol;
[0049] Figure 2 It is the gas chromatography-mass spectrum of 1,2-propylene glycol;
[0050] Figure 3 It is the gas chromatography-mass spectrum of 1,3-propanediol;
[0051] Figure 4 is the gas chromatography-mass spectrum of butanediol;
[0052] Figure 5 is the gas chromatography-mass spectrum of methylpropanediol;
[0053] Figure 6 It is the gas chromatography-mass spectrum of 1,2-pentanediol;
[0054] Figure 7 It is the gas chromatography-mass spectrum of dipropylene glycol;
[0055] Figure 8 is the gas chromatography-mass spectrum of glycerol;
[0056] Fig. 9 It is the gas chromatography-mass spectrum of 1,2-hexanediol. DETAILED DESCRIPTION
[0057] After extensive and in-depth research, the inventors have successfully separated the isomers in multiple cosmetics by screening characteristic ion pairs combined with the optimization of chromatographic examination. The isomers can be used to simultaneously analyze the contents of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol in cosmetics. The detection method is simple to operate, fast to analyze, highly specific, and has a high degree of separation. The method can be used as a detection method for polyol moisturizers in cosmetics, and provides technical support for the analysis of moisturizing functional raw materials in cosmetics.
[0058] To make the purpose, technical scheme and advantages of the embodiments of the present application clearer, the present application is further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present application and are not intended to limit the scope of the present application. The experimental methods in the following examples that do not specify specific conditions are usually based on normal conditions or according to the conditions recommended by the manufacturer. Unless otherwise specified, percentages and parts are weight percentages and weight parts. The experimental materials and reagents used in the following examples can be obtained from commercial channels unless otherwise specified.
[0059] Unless otherwise specified, the technical and scientific terms used herein have the same meaning as commonly understood by ordinary technicians in the technical field to which the application belongs. It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments of the present application.
[0060] Example 1
[0061] 1. Instruments, reagents and materials
[0062] Ethylene glycol standards were purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. with a purity of 99.5%; 1,2-propylene glycol standards were purchased from Shanghai Anpu Experimental Technology Co., Ltd. with a purity of 99.5%; 1,3-propylene glycol standards were purchased from Shanghai Anpu Experimental Technology Co., Ltd. with a purity of 99.5%; butanediol standards were purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. with a purity of 99.0%; methylpropanediol standards were purchased from Shanghai MacLean Biochemical Technology Co., Ltd. with a purity of 98.0%; 1,2-pentanediol standards were purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. with a purity of 98.0%; dipropylene glycol standards were purchased from Shanghai MacLean Biochemical Technology Co., Ltd. with a purity of 95.0%; propylene glycol standards were purchased from Shanghai MacLean Biochemical Technology Co., Ltd. with a purity of 99.7%; 1,2-hexanediol standards were purchased from Shanghai Anpu Experimental Technology Co., Ltd. with a purity of 96.0%. Methanol was purchased from Thermo Fisher Scientific Inc., chromatographic grade; n-hexane was purchased from Thermo Fisher Scientific Inc., chromatographic grade; acetone was purchased from Thermo Fisher Scientific Inc., chromatographic grade; water was ultrapure water. Shimadzu GC-2010plus gas chromatograph, Shimadzu GCMS-TQ8040 mass spectrometer, IKAVORTEX4 vortexer, Eppendorf 5810R centrifuge, Swiss Mettler-Toledo electronic balance, American EMERSON ultrasonic instrument. 0.22 μm microporous filter membrane (nylon 6, Navigator).
[0063] 2. Testing process
[0064] Preparation of standard products: Accurately weigh 100 mg each of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol, and 1,2-hexanediol standard products, place them in the same 10 mL volumetric flask, dissolve them in methanol, and make up to the mark. Shake well to use as standard stock solutions of the nine polyols.
[0065] Preparation of standard solution: Accurately pipette an appropriate amount of standard stock solution and dilute it with methanol to make 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 preparation:
[0067] Liquid water-based, creams, lotions, and powder samples: Accurately weigh 0.25 g (accurate to 0.0001 g) of the sample and 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 the scale, vortex to mix, centrifuge at 10,000 r / min for 5 minutes, take an appropriate amount of supernatant, filter through a 0.22 μm organic filter membrane, and set aside the filtrate.
[0068] 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, then add 3 mL of methanol, vortex for 1 min, centrifuge at 4000 r / min for 5 min, pipette the lower layer solution into a 25 mL stoppered colorimetric tube, extract the upper layer with 3 mL of methanol repeatedly, combine the two solutions, add methanol to the scale, vortex to mix, centrifuge at 10000 r / min for 5 min, take an appropriate amount of supernatant, pass it through a 0.22 μm organic filter membrane, and set the filtrate aside.
[0069] Wax-based samples: Accurately weigh 0.25 g of sample (accurate to 0.0001 g), place 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 seconds and mix thoroughly, ultrasonicate for 10 minutes, cool to room temperature, add methanol to the scale, vortex to mix, centrifuge at 10000 r / min for 5 minutes, take an appropriate amount of supernatant, filter through a 0.22 μm organic filter membrane, and set aside the filtrate.
[0070] Detection: The series of standard solutions in (2) and the filtrate in (3) are respectively injected into a gas chromatograph for quantitative analysis.
[0071] 1) Gas chromatography parameters
[0072] Chromatographic column: DB-624 gas chromatography 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] Program temperature rise: initial temperature 50°C, hold for 2 min, increase the temperature to 140°C at 10°C / min, hold for 1 min, increase the temperature to 185°C at 8°C / min, hold for 5 min, increase the temperature to 230°C at 20°C / min, hold for 1.13 min.
[0074] 2) Mass spectrometry parameters
[0075] Ionization 230 mode: EI; ion source temperature: 230°C, mass spectrometer interface: 240°C, solvent delay: 5 min, detector voltage: tuning voltage, detection mode: selected ion monitoring (SIM), compound information is shown in Table 3. The ions with higher response and less interference were used as quantitative ions, and the rest were used as qualitative ions.
[0076] Table 3 GC-MS parameters of 9 polyols including methyl propylene glycol
[0077]
[0078] Note: * is the quantitative ion
[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 of 9 polyols including methyl propylene glycol
[0081]
[0082] Test results see Figure 1-9 .
[0083] 3. Test condition optimization
[0084] 3.1 Column selection and temperature program optimization
[0085] During the analysis, the compounds are similar in structure, retention time and molecular weight, which makes it easy to produce the same fragments. In order to ensure the accurate identification and quantification of the compounds, it is necessary to ensure that the components are effectively separated on the chromatographic column. DB-624 column (30m×0.25mm×1.4μm), DB-5MS column (30m×0.25mm×0.25μm) and INNOWAX column (30m×0.25mm×0.25μm) were used to test the separation effect.
[0086] The results show that the DB-5MS column is a non-polar column and is not suitable for analyzing highly polar compounds such as propylene glycol and glycerol, resulting in peak tailing. A good peak shape can be obtained by using a highly polar INNOWAX column, but 1,2-pentanediol and 1,3-propylene glycol cannot be completely separated. Selecting a DB-624 column suitable for volatile compounds can obtain a good peak shape. By adjusting the program temperature, lowering the initial temperature to 50°C, and slowly increasing the temperature, the 9 compounds can achieve good separation and peak shape.
[0087] 3.2 Selection of ion pairs
[0088] Since the molecular weights of the nine compounds are concentrated between 62 and 135, there are two pairs of isomers, 1,2-propylene glycol and 1,3-propylene glycol, and butanediol and methylpropanediol. In addition to ensuring the effective separation of chromatographic peaks, it is necessary to try to select different characteristic ions to ensure the accuracy of qualitative and quantitative analysis. The characteristic ions of 1,2-propylene glycol and 1,3-propylene glycol are 45, 61, 29, 57, 28, and 31, respectively; the characteristic ions of butanediol and methylpropanediol are 43, 72, 57, 42, 57, and 31, respectively.
[0089] 3.3 Choice of solvent
[0090] Methanol, acetonitrile and acetone were used as solvents respectively, and good chromatographic peaks were obtained on the DB-624 column, and there was no significant difference in the response of the 9 components. At the same time, the three solvents were investigated as sample extraction and dispersion solvents, and the recovery rates all met the requirements. Considering the toxicity of acetonitrile and acetone solvents, methanol was finally selected as the standard solvent and sample extraction solvent.
[0091] 4. Precision and stability investigation
[0092] The precision of the instrument was investigated by continuous injection of 6 injections of mixed standard solutions with concentrations of 100μg / mL, 200μg / mL, and 400μg / mL, and the results showed that the peak area RSD was less than 5%, indicating that the precision of the instrument was good. The mixed standard solutions with concentrations of 100μg / mL, 200μg / mL, and 400μg / mL and the blank matrix spiked solution were measured on the first, second, third, fourth, and fifth days, respectively, and the peak area RSD was less than 5%, indicating that the 9 polyols could remain stable within 5 days.
[0093] Example 2
[0094] Five commercially available cosmetic matrices were used as test objects, spiked with 10 mg / g, 20 mg / g and 40 mg / g, and parallel tests (n=6) were performed to determine the recovery rate and relative deviation (RSD%). The results are shown in Table 5. The results show that the recovery rate of the nine components under high, medium and low spike concentration conditions ranged from 95.68% to 105.57%, and the relative deviation (RSD) (n=6) was from 1.40% to 7.25%, indicating that the recovery rate of this method is good.
[0095] Table 5 Recovery results (n=6)
[0096]
[0097]
[0098] Example 3
[0099] Applying this detection method, we selected commercially available products containing polyol moisturizers on their labels, including liquid oil-based, creams and lotions, wax-based, powders, and liquid water-based moisturizing cosmetics (toner, essence, face cream, loose powder, essential oil, etc.). A total of 20 batches were tested in accordance with the law, of which 11 batches were found to contain polyol moisturizers. The test results are detailed in the table below.
[0100] Table 6 Positive sample results
[0101]
[0102] The above description shows and describes 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 by the above embodiments. The above embodiments are only preferred embodiments of the present invention and cannot be used to limit the scope of the present invention. That is, equivalent changes and modifications made according to the patent scope of the present invention and the content of the specification should still be within the scope of the present invention. The scope of protection required by the present invention is defined by the attached claims and their equivalents.
[0103] Those skilled in the art will appreciate that the above-mentioned embodiments are specific examples for implementing the present application, and in actual applications, various changes may be made thereto in form and detail without departing from the spirit and scope of the present application.
Claims
1. A method for simultaneously detecting multiple polyols in cosmetics, characterized in that: The method comprises the steps of: using a gas chromatograph-mass spectrometer to simultaneously detect the contents of 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol and methylpropylene glycol in the cosmetics to be tested, wherein the mass spectrometry conditions of the gas chromatograph-mass spectrometer include: selecting 45m / z, 61m / z and 29m / z as characteristic ions of 1,2-propylene glycol; 57 m / z , 28 m / z , and 31 m / z were selected as characteristic ions of 1,3-propanediol; Selecting 43m / z, 72m / z, and 57m / z as characteristic ions of butanediol; and 42 m / z, 57 m / z, and 31 m / z were selected as characteristic ions of methylpropanediol.
2. The method according to claim 1, characterized in that The method can simultaneously detect the contents of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol and 1,2-hexanediol.
3. The method according to claim 2, characterized in that The mass spectrometry conditions of the gas chromatography-mass spectrometer include: selecting 31m / z as the qualitative ion of ethylene glycol, and selecting 43m / z and 62m / z as the quantitative ions of ethylene glycol; Select 45*m / z as the qualitative ion of 1,2-propylene glycol, and select 61m / z and 29m / z as the quantitative ions; Select 57*m / z as the qualifier ion of 1,3-propylene glycol, and 28m / z and 31m / z as the quantitative ions of 1,3-propylene glycol; Select 43*m / z as the qualitative ion of butanediol, and select 72m / z and 57m / z as the quantitative ions of butanediol; Select 42* as the methylpropanediol qualitative ion, and select 57m / z and 31m / z as the methylpropanediol quantitative ions; Select 55*m / z as the qualifier ion for 1,2-pentanediol, and select 73m / z and 43m / z as the quantitative ions for 1,2-pentanediol; Select 45*m / z as the DPG qualitative ion, and select 89m / z and 59m / z as the DPG quantitative ions; Select 61*m / z as the glycerol qualitative ion, and select 43m / z and 31m / z as the glycerol quantitative ions; and / or 69*m / z was selected as the qualifier ion for 1,2-hexanediol, and 87m / z and 41m / z were selected as the quantitative ions for 1,2-hexanediol.
4. The method according to claim 3, characterized in that The chromatographic conditions of the gas chromatography-mass spectrometry instrument include: selecting a medium polarity chromatographic column as the analytical column, preferably a DB-624 chromatographic column.
5. The method according to claim 4, characterized in that The chromatographic conditions of the gas chromatograph-mass spectrometer include: setting a programmed temperature increase, with an initial temperature of approximately 50°C, then increasing the temperature to 140°C at 10°C / min and holding it for at least 1 min, increasing the temperature to 185°C at 8°C / min and holding it for at least 5 min, and increasing the temperature to 230°C at 20°C / min and holding it for at least 1.13 min.
6. The method according to claim 1, characterized in that The cosmetic to be tested is selected from at least one of liquid water-based, cream and lotion-based, liquid oil-based, wax-based, and powder-based.
7. The method according to claim 6, characterized in that The method further comprises the step of selecting a suitable pre-treatment method according to the matrix type of the cosmetic to be tested.
8. The method according to claim 7, characterized in that When the cosmetics to be tested are liquid water-based, cream, lotion or powder, the pretreatment method includes the steps of taking the sample to be tested, adding methanol to dissolve it, and then taking the supernatant for testing; And / or, when the cosmetic to be tested is a liquid oil-based cosmetic, the pretreatment method includes the steps of first adding n-hexane to the sample to be tested and then adding methanol to dissolve the sample and then taking the supernatant for testing; And / or, when the cosmetics to be tested are wax-based, the pretreatment method includes the steps of first adding tetrahydrofuran to the sample to be tested and then adding methanol to dissolve it, and then taking the supernatant for testing.
9. The method according to claim 7, characterized in that After selecting a suitable pre-treatment method according to the matrix type of the cosmetic to be tested, the method further comprises the following steps: Detect ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol and 1,2-hexanediol standard solutions and draw standard curves; The cosmetics to be tested are detected, and the contents of ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, butylene glycol, methyl propanediol, 1,2-pentanediol, dipropylene glycol, glycerol and 1,2-hexanediol in the cosmetics to be tested are obtained according to the standard curve.
10. The method according to claim 1, characterized in that The cosmetics are selected from at least one of toner, body lotion, essence, face cream, loose powder, essential oil, facial mask, hand mask, eye patch, spray, lipstick, lip mask, sunscreen, primer, liquid foundation, facial cleanser, hand cream, shampoo, conditioner, hair essential oil, shower gel, nail polish, and body oil.