CN112684046B - Method for measuring components of oil and fat in cosmetics - Google Patents

Method for measuring components of oil and fat in cosmetics Download PDF

Info

Publication number
CN112684046B
CN112684046B CN202011512226.1A CN202011512226A CN112684046B CN 112684046 B CN112684046 B CN 112684046B CN 202011512226 A CN202011512226 A CN 202011512226A CN 112684046 B CN112684046 B CN 112684046B
Authority
CN
China
Prior art keywords
standard
solution
stock solution
cosmetics
oil
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202011512226.1A
Other languages
Chinese (zh)
Other versions
CN112684046A (en
Inventor
裴丽娟
冯俊
张冬琴
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Microspectrum Detection Technology Co ltd
Original Assignee
Shanghai Microspectrum Detection Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Microspectrum Detection Technology Co ltd filed Critical Shanghai Microspectrum Detection Technology Co ltd
Priority to CN202011512226.1A priority Critical patent/CN112684046B/en
Publication of CN112684046A publication Critical patent/CN112684046A/en
Application granted granted Critical
Publication of CN112684046B publication Critical patent/CN112684046B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to a method for detecting components of cosmetics, in particular to a method for detecting components of oil in cosmetics. The method for measuring the components of the oil and fat in the cosmetics is researched, wherein the oil and fat comprises cetyl ethyl hexanoate, isooctyl palmitate, glycerol triethyl hexanoate, glycerol tricaprylate, neopentyl glycol diheptanoate, cetyl stearyl alcohol, isononyl isononanoate, squalane, glycerol caprylate, isopropyl myristate, silicone oil and VE acetate; the method comprises the following steps: preparing a sample solution to be detected; (2) preparing a standard solution stock solution; (3) preparing a mixed standard working solution; (4) gas chromatography-mass spectrometer analysis; and (5) analyzing results. The method for detecting the grease in the cosmetics has the characteristics of simplicity, convenience, rapidness and sensitivity.

Description

Method for measuring components of oil and fat in cosmetics
Technical Field
The invention relates to a method for detecting components of cosmetics, in particular to a method for detecting components of oil in cosmetics.
Background
In cosmetics, fats and oils are frequently used raw materials, and fats and oils are extracted from natural fats and oils and raw materials, and are obtained by processing, synthesizing and modifying natural fats and oils, and have properties of chemical stability, skin irritation and better skin absorbability as compared with natural fats and oils. The variety and the content of the oil in the cosmetics influence the irritation of skin and the skin absorbability to a great extent, so that the establishment of a detection method which can accurately, conveniently and quantitatively detect the oil in the cosmetics is necessary, and the monitoring of the addition amount of the oil in the field of the cosmetics is facilitated, so that the safety and the effective use of the cosmetics are ensured.
Disclosure of Invention
In order to solve the above-mentioned technical problems, the first aspect of the present invention provides a method for measuring the composition of oils and fats in cosmetics, the oils and fats including cetyl ethylhexanoate, isooctyl palmitate, triethylhexanoin, tricaprylin, neopentyl glycol diheptanoate, cetearyl alcohol, isononyl isononanoate, squalane, caprylic glyceride, isopropyl myristate, silicone oil, VE acetate; comprises the steps of
(1) Preparing a sample solution to be tested: taking a cosmetic sample, and dissolving the cosmetic sample in an organic solvent;
(2) Preparation of standard solution stock solution: preparing a standard solution stock solution A containing a glycerol caprylate standard substance and a standard solution stock solution B containing cetyl ethyl hexanoate, isooctyl palmitate, glycerol triethylhexanoate, neopentyl glycol diheptanoate, cetyl stearyl alcohol, isononyl isononanoate, squalane, glycerol tricaprylate, isopropyl myristate, silicone oil and VE acetate respectively;
(3) Preparation of mixed standard working solution: respectively preparing a mixed standard stock solution A and a mixed standard stock solution B by using the standard solution stock solution A and the standard solution stock solution B; diluting the mixed standard stock solution A and the mixed standard stock solution B in a grade-B manner to obtain a mixed standard working solution A and a mixed standard working solution B with different concentrations;
(4) Gas chromatography-mass spectrometer analysis: detecting and analyzing the mixed standard working solution and the sample solution by using a gas chromatography-mass spectrometer;
(5) And (4) analyzing results: and establishing a standard curve and verifying the method.
As a preferred embodiment of the present invention, the organic solvent includes chloroform.
As a preferred technical solution of the present invention, the organic solvent further comprises a small molecule alcohol; the volume ratio of the small molecular alcohol to the trichloromethane is (0.8-1.2): 1.
as a preferable technical scheme of the invention, the small molecular polyol is one of methanol, ethanol and isopropanol.
As a preferable technical scheme of the invention, the concentration of the standard solution stock solution A is 40000mg/L, and the concentration of the standard solution stock solution B is 25000mg/L.
As a preferable technical scheme of the invention, the concentration of the mixed standard stock solution A is 4000mg/L, and the concentration of the mixed standard stock solution B is 1000mg/L.
As a preferable technical scheme of the invention, the concentration of the mixed standard stock solution A is 4000mg/L, and the mixed standard working solution comprises 4 different concentrations; of the 4 different concentrations, the concentrations of the mixed standard working solution A were 200mg/L, 400mg/L, 800mg/L, and 1600mg/L, respectively, and the concentrations of the mixed standard working solution B were 50mg/L, 100mg/L, 200mg/L, and 400mg/L, respectively.
As a preferred technical solution of the present invention, the chromatographic parameters of the gas chromatography are: a chromatographic column: HP-5MS (30 m × 0.25mm × 0.25 μm); carrier gas: high purity helium gas; sample inlet temperature: 250 ℃; the split ratio is as follows: 25; column temperature procedure: keeping the temperature at 125 ℃ for 3min, heating to 280 ℃ at the heating rate of 15 ℃/min, and keeping the temperature for 4min; the temperature is raised to 305 ℃ at a speed of 30 ℃/min and is kept for 8min.
As a preferable technical scheme of the invention, the flow rate of the gas chromatography is 0.8-1.2 mL/min.
As a preferred technical solution of the present invention, the parameters of the mass spectrometer are: mass spectrometry interface temperature: 280 ℃; solvent retardation: 3min; an ion source: 230 ℃; a fourth-stage rod: 150 ℃; scanning: scan & Sim Scan.
Has the advantages that:
1. a gas chromatography/mass spectrometry detection method for the oil in the cosmetics such as cetyl ethyl hexanoate, isooctyl palmitate, glycerol triethyl hexanoate, glycerol tricaprylate, neopentyl glycol diheptanoate, cetyl stearyl alcohol, isononyl isononanoate, squalane, glycerol caprylate, isopropyl myristate, silicone oil and VE acetate 12 is established, and the simultaneous detection of the oil in 12 is realized;
2. gas chromatography/mass spectrometry analysis conditions for simultaneously measuring 12 kinds of grease are established, and separation and qualitative and quantitative detection of 12 kinds of grease are completed within 27 min;
3. the relative error of the research of the established method for measuring the components of the grease in the cosmetics is within 12 percent, and the quantitative result is good;
4. the recovery rate of the research of the established method for measuring the components of the grease in the cosmetics is good, the RSD is less than 10 percent, and the repeatability is good;
5. the method for measuring the grease in the cosmetics has the characteristics of simplicity, convenience, rapidness and sensitivity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a gas chromatogram of a blank test and a mixed standard test.
Detailed Description
The present invention will be more readily understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
As used herein, the term "consisting of 8230; preparation" is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of 8230comprises" excludes any non-specified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of 8230is present in a clause of the claim body, rather than immediately after the subject matter, it defines only the elements described in that clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "either" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
In order to solve the above technical problems, the first aspect of the present invention provides a method for measuring the composition of oils and fats in cosmetics, the oils and fats including cetyl ethylhexanoate, isooctyl palmitate, triethylhexanoate, tricaprylin, neopentyl glycol diheptanoate, cetearyl alcohol, isononyl isononanoate, squalane, caprylic glyceride, isopropyl myristate, silicone oil, VE acetate; comprises the steps of
(1) Preparing a sample solution to be detected: taking a cosmetic sample, and dissolving the cosmetic sample in an organic solvent;
(2) Preparation of standard solution stock solution: preparing a standard solution stock solution A containing a caprylic glyceride standard and a standard solution stock solution B respectively containing cetyl ethyl hexanoate, isooctyl palmitate, glycerol triethyl hexanoate, neopentyl glycol diheptanoate, cetyl stearyl alcohol, isononyl isononanoate, squalane, tricaprylin, isopropyl myristate, silicone oil and VE acetate;
(3) Preparation of mixed standard working solution: respectively preparing a mixed standard stock solution A and a mixed standard stock solution B by using the standard solution stock solution A and the standard solution stock solution B; diluting the mixed standard stock solution A and the mixed standard stock solution B in a grade-B manner to obtain a mixed standard working solution A and a mixed standard working solution B with different concentrations;
(4) Gas chromatography-mass spectrometer analysis: detecting and analyzing the mixed standard working solution and the sample solution by using a gas chromatography-mass spectrometer;
(5) And (4) analyzing results: and establishing a standard curve and verifying the method.
Figure 127606DEST_PATH_IMAGE001
Specifically, the research and the steps of the method for measuring the components of the oil and fat in the cosmetics are as follows:
1. standard substance and sample information
1.1 Standard substance: the information of the grease standards in 12 is shown in table 1:
TABLE 1
Figure 779167DEST_PATH_IMAGE002
1.2 Sample formulations were developed as shown in table 2:
TABLE 2
Figure 27746DEST_PATH_IMAGE003
2. Solution preparation
2.1 Preparation of sample solution to be tested
Taking a research and development sample, and dissolving the research and development sample in an organic solvent.
In one embodiment, the organic solvent comprises chloroform.
In a preferred embodiment, the organic solvent further comprises a small molecule alcohol; the volume ratio of the small molecular alcohol to the trichloromethane is (0.8-1.2): 1; the volume ratio of the micromolecular alcohol to the trichloromethane is 1:1.
in a more preferred embodiment, the small molecule alcohol is one of methanol, ethanol and isopropanol; further preferably, the small molecule alcohol is methanol.
Generally, when the cosmetics are analyzed by a gas chromatography-mass spectrometer, a solvent is needed to dissolve the cosmetics firstly, and in the field, the solubility of trichloromethane is better, but researches show that the accuracy of detection is reduced by using the trichloromethane alone, and the trichloromethane and methanol are used, particularly the volume ratio is 1: chloroform of 1 and methanol were more effective in dissolving the sample.
Most of the synthetic lipid in the cosmetics measured by the invention is alcohol ester substances, the dissolving effect of the organic solvent containing micromolecule alcohol is better, particularly, the methanol is micromolecule alcohol with stronger polarity, the solvent property of the trichloromethane is very weak, the chloroform is equivalent to a nonpolar molecule, and the solvent with strong polarity and very weak polarity is adopted to dissolve a cosmetic sample, so that the synthetic lipid can well interact with the polar and nonpolar synthetic lipids in the cosmetics, and the accuracy of detection is reduced and the interference of impurities is improved.
Specifically, about 0.1g (accurate to 0.0001 g) of a research and development sample is taken and dissolved in a 10mL volumetric flask, and the volume is determined to the scale by methanol-chloroform (volume ratio is 1.
2.2 Preparation of stock solutions of Standard solutions
Preparing a standard solution stock solution A containing a caprylic glyceride standard and a standard solution stock solution B respectively containing cetyl ethyl hexanoate, isooctyl palmitate, glycerol triethyl hexanoate, neopentyl glycol diheptanoate, cetyl stearyl alcohol, isononyl isononanoate, squalane, tricaprylin, isopropyl myristate, silicone oil and VE acetate; among them, there were 1 group of stock solutions of standard solution A and 11 group of stock solutions of standard solution B.
In one embodiment, the solvent for preparing the stock solution of standard solution is chloroform.
In one embodiment, the concentration of the standard solution stock solution A is 40000mg/L and the concentration of the standard solution stock solution B is 25000mg/L.
Specifically, 0.4g (to 0.0001 g) of the glyceryl caprylate standard is accurately weighed, 0.25g (to 0.0001 g) of the other 11 standards is weighed in a 10mL volumetric flask, chloroform is used for metering to a scale, and the standard solution stock solution A40000mg/L and the standard solution stock solution B25000mg/L are respectively prepared.
2.3 Preparation of Mixed stock solutions
In one embodiment, the concentration of mixed standard stock solution A is 4000mg/L and the concentration of mixed standard stock solution B is 1000mg/L.
Specifically, a standard solution stock solution A2.5mL is accurately sucked by an air-tight injector, 1.00mL of each standard solution stock solution B is placed in a 25mL volumetric flask, chloroform is used for diluting to a constant volume, and a mixed standard stock solution of a mixed standard stock solution A4000mg/L and a mixed standard stock solution B1000 mg/L is prepared.
2.3 Mixed Standard working solution preparation
Respectively preparing a mixed standard stock solution A and a mixed standard stock solution B by using the standard solution stock solution A and the standard solution stock solution B; diluting the mixed standard stock solution A and the mixed standard stock solution B in a grade-B manner to obtain a mixed standard working solution A and a mixed standard working solution B with different concentrations;
as a preferable technical scheme of the invention, the concentration of the mixed standard stock solution A is 4000mg/L, and the mixed standard working solution comprises 4 different concentrations; of the 4 different concentrations, the concentrations of the mixed standard working solution A were 200mg/L, 400mg/L, 800mg/L, and 1600mg/L, respectively, and the concentrations of the mixed standard working solution B were 50mg/L, 100mg/L, 200mg/L, and 400mg/L, respectively.
Specifically, the mixed quasi-stock solution in 2.3 is used as a mother solution, chloroform is used for diluting to a constant volume, the concentrations of the mixed standard working solution A are respectively 200mg/L, 400mg/L, 800mg/L and 1600mg/L, and the concentrations of the mixed standard working solution B are respectively 50mg/L, 100mg/L, 200mg/L and 400mg/L.
3. Parameters of the instrument
In one embodiment, the chromatographic parameters of the gas chromatograph are: a chromatographic column: HP-5MS (30 m × 0.25mm × 0.25 μm); carrier gas: high purity helium gas; sample inlet temperature: 250 ℃; the split ratio is as follows: 25; column temperature procedure: keeping the temperature at 125 ℃ for 3min, heating to 280 ℃ at the heating rate of 15 ℃/min, and keeping the temperature for 4min; the temperature is raised to 305 ℃ at a speed of 30 ℃/min and is kept for 8min.
In a preferred embodiment, the flow rate of the gas chromatograph is 0.8 to 1.2 mL/min; further preferably, the flow rate of the gas chromatograph is 1 mL/min.
In one embodiment, the parameters of the mass spectrometer are: mass spectrum interface temperature: 280 ℃; solvent retardation: 3min; an ion source: 230 ℃; a fourth-stage rod: 150 ℃; scanning: scan & Sim Scan.
Specifically, the chromatographic parameters of the gas chromatography are shown in table 3; the mass spectrometer parameters are shown in table 4.
TABLE 3
Figure 829479DEST_PATH_IMAGE004
TABLE 4
Figure 83000DEST_PATH_IMAGE005
In order to verify the research feasibility and accuracy of the method for determining the components of the oil in the cosmetics, the invention carries out the following verification:
4. solubility of sample
1. Methanol and methanol = chloroform (1) respectively dissolve the 12 th standard, and the sample is completely dissolved.
5. Selectivity is
5.1 Blank test: blank tests were carried out in the same manner as above except that no sample was added.
5.2 And (3) mixing standard test: the mixed standard working solution was tested according to the procedure described above.
The gas chromatograms of the blank test and the mixed standard test are shown in fig. 1.
From fig. 1, it can be seen that no target peak appears in the blank test, which indicates that no interference is generated in the sample quantification, and the target appearing in the sample can be directly quantified.
6. Linearity
And (3) according to the standard solution of the series of concentrations of the substances in the step 2 and the instrument test conditions in the step 3, performing test analysis through a gas chromatography-mass spectrometer, recording a chromatogram and a corresponding peak area, and drawing a fitting curve by taking the concentration of the mixed standard solution as a horizontal coordinate and the peak area as a vertical coordinate. And calculating the linear range and the correlation coefficient of the linear range. The data results are shown in Table 5.
TABLE 5
Figure 843145DEST_PATH_IMAGE006
The results show that: the target has good linear relation, and the fitting correlation coefficient R2 is more than or equal to 0.990.
7. Detection limit and quantification limit
And determining the 3-time signal-to-noise ratio as the detection limit of the instrument, wherein the target object is quantified by an SIM (subscriber identity module) ion extraction method. Table 6 shows the instrumental detection limits for 12 targets.
TABLE 6
Figure 782282DEST_PATH_IMAGE007
The results show that: the limit of quantitation is less than the linear low point.
8. Rate of accuracy
The research and development sample is taken as a test sample, the quantitative result is compared with the actual content of the toothpaste skin target object, and the relative error is calculated and is shown in table 7.
TABLE 7
Figure 450024DEST_PATH_IMAGE008
The results show that: the relative error of the quantitative result of the research and development sample is within 12 percent, and the quantitative result is good.
9. Repeatability of
According to the research and development sample testing method, according to the measuring conditions in the instrument parameters, the sample solution to be tested which is prepared in parallel is sequentially led into a gas chromatography-mass spectrometer for measurement, the peak area of each substance is recorded, and the specific result is shown in table 8.
TABLE 8
Figure 587744DEST_PATH_IMAGE009
The results show that: the recovery rate of the developed sample is good, the RSD is less than 10%, and the stability is good.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
Examples
Example 1
Embodiment 1 of the present invention specifically provides a study on a method for measuring a component of oil or fat in a cosmetic, comprising the steps of:
1. standard substance and sample information
1.1 Standard substance: the information on the grease standards in 12 is shown in table 9:
TABLE 9
Figure 49950DEST_PATH_IMAGE010
1.2 Sample formulations were developed as shown in table 10:
TABLE 10
Figure 37235DEST_PATH_IMAGE011
2. Solution preparation
2.1 Preparation of sample solution to be tested
Taking about 0.1g (accurate to 0.0001 g) of a developed sample to be dissolved in a 10mL volumetric flask, adding methanol-trichloromethane (volume ratio is 1;
2.2 Preparation of stock solutions of Standard solutions
Accurately weighing 0.4g (accurate to 0.0001 g) of a glyceryl caprylate standard substance, weighing 0.25g (accurate to 0.0001 g) of the other 11 standard substances in a 10mL volumetric flask, metering the volume to scale by using trichloromethane, and respectively preparing a standard solution stock solution A40000mg/L and a standard solution stock solution B25000mg/L;
2.3 Preparation of Mixed Standard stock solutions
Accurately sucking 2.5mL of standard solution stock solution A by using an airtight syringe, putting 1.00mL of each standard solution stock solution B in a 25mL volumetric flask, diluting with trichloromethane to a constant volume, and preparing mixed standard stock solution of mixed standard stock solution A4000mg/L and mixed standard stock solution B1000 mg/L;
2.3 Mixed Standard working solution preparation
Taking the mixed quasi-stock solution in the step 2.3 as mother liquor, diluting with trichloromethane to a constant volume, and preparing mixed standard working solutions A with the concentrations of 200mg/L, 400mg/L, 800mg/L and 1600mg/L respectively, and mixed standard working solutions B with the concentrations of 50mg/L, 100mg/L, 200mg/L and 400mg/L respectively;
3. parameters of the instrument
The chromatographic parameters of the gas chromatograph are shown in table 3; the mass spectrometer parameters are shown in table 4:
TABLE 3
Figure 243088DEST_PATH_IMAGE012
TABLE 4
Figure 235315DEST_PATH_IMAGE013
4. Gas chromatography-mass spectrometer analysis
Detecting and analyzing the mixed standard working solution and the sample solution by using a gas chromatography-mass spectrometer;
the final analysis results gave: the method can be used for carrying out qualitative and quantitative analysis on the grease in the cosmetics, the peaks of target products can be well distinguished, and the method has good selectivity and sharp peak shape.
Example 2
Example 2 of the present invention specifically provides a study on a method for measuring a component of an oil or fat in a cosmetic, and the specific embodiment thereof is the same as example 1 except that the organic solvent is chloroform.
The final analysis results gave: the accuracy is reduced, the selectivity is reduced, and the separation is not facilitated.
Example 3
Example 3 of the present invention specifically provides a study on a method for measuring a component of an oil or fat in a cosmetic, and the specific embodiment thereof is the same as example 1 except that the organic solvent is methanol.
The final analysis results gave: the accuracy is reduced, the selectivity is reduced, and the separation is not facilitated.
Example 4
Example 4 of the present invention specifically provides a study on a method for measuring a component of an oil or fat in a cosmetic, and the specific embodiment thereof is the same as example 1 except that the split ratio is 35.
The final analysis results gave: the peak shape is wider and tailing phenomenon exists.
Example 5
Example 5 of the present invention provides a study on a method for measuring components of fats and oils in cosmetics, and the present invention is similar to example 1 except that the flow rate of gas chromatography is 1.5 mL/min.
The final analysis results gave: the selectivity is reduced and separation is not facilitated.
Example 6
Example 6 of the present invention specifically provides a study on a method for measuring a component of an oil or fat in a cosmetic, and the specific embodiment is the same as example 1, except that the column temperature program is: keeping the temperature at 125 ℃ for 3min, increasing the temperature to 305 ℃ at the heating rate of 15 ℃/min, and keeping the temperature for 10.2min.
The final analysis results gave: the target peak is difficult to distinguish.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as can be conceived and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Where the claims recite a range of values, such ranges are intended to include all sub-ranges subsumed therein, and variations within the ranges are intended to be encompassed by the claims as appended hereto where possible.

Claims (5)

1. A method for measuring the composition of oils and fats in cosmetics, characterized in that the oils and fats include cetyl ethylhexanoate, isooctyl palmitate, triethylhexanoate, tricaprylin, neopentyl glycol diheptanoate, cetearyl alcohol, isononyl isononanoate, squalane, glyceryl caprylate, isopropyl myristate, silicone oil and VE acetate; the method comprises the following steps:
(1) Preparing a sample solution to be detected: taking a cosmetic sample, and dissolving the cosmetic sample in an organic solvent;
(2) Preparation of standard solution stock solution: preparing a standard solution stock solution A containing a caprylic glyceride standard and a standard solution stock solution B respectively containing cetyl ethyl hexanoate, isooctyl palmitate, glycerol triethyl hexanoate, neopentyl glycol diheptanoate, cetyl stearyl alcohol, isononyl isononanoate, squalane, tricaprylin, isopropyl myristate, silicone oil and VE acetate;
(3) Preparation of standard working solution: respectively preparing a standard stock solution A and a mixed standard stock solution B by using the standard stock solution A and the standard stock solution B; diluting the standard stock solution A and the mixed standard stock solution B in a grade-B manner to obtain standard working solutions A and mixed standard working solutions B with different concentrations;
(4) Gas chromatography-mass spectrometer analysis: detecting and analyzing the standard working solution and the sample solution by using a gas chromatography-mass spectrometer;
(5) And (4) analyzing results: establishing a standard curve and verifying the method;
the organic solvent comprises chloroform;
the organic solvent also comprises small molecular alcohol; the volume ratio of the small molecular alcohol to the trichloromethane is (0.8-1.2): 1;
the chromatographic parameters of the gas chromatograph are as follows: a chromatographic column: HP-5MS with the specification of 30m multiplied by 0.25mm multiplied by 0.25 mu m; carrier gas: high purity helium gas; sample inlet temperature: 250 ℃; the split ratio is as follows: 25; column temperature procedure: keeping the temperature at 125 ℃ for 3min, heating to 280 ℃ at the heating rate of 15 ℃/min, and keeping the temperature for 4min; heating to 305 deg.C at 30 deg.C/min, and maintaining for 8min;
the flow rate of the gas chromatography is 0.8-1.2 mL/min;
the parameters of the mass spectrometer are: mass spectrum interface temperature: 280 ℃; solvent retardation: 3min; an ion source: 230 ℃; a fourth-stage rod: 150 ℃; scanning: scan & Sim Scan.
2. The method for measuring the composition of an oil or fat in a cosmetic according to claim 1, wherein the small-molecular alcohol is one of methanol, ethanol, and isopropyl alcohol.
3. The method of measuring the content of a fat or oil in a cosmetic according to claim 1, wherein the stock solution A of the standard solution has a concentration of 40000mg/L and the stock solution B of the standard solution has a concentration of 25000mg/L.
4. The method for measuring the composition of fats and oils in cosmetics according to claim 1, wherein the concentration of the standard stock solution A is 4000mg/L and the concentration of the mixed standard stock solution B is 1000mg/L.
5. The method for measuring the composition of fats and oils in cosmetics according to claim 1, wherein the concentration of said standard stock solution A is 4000mg/L, and said standard working solution comprises 4 different concentrations; of the 4 different concentrations, the concentrations of the standard working solution A were 200mg/L, 400mg/L, 800mg/L, and 1600mg/L, respectively, and the concentrations of the mixed standard working solution B were 50mg/L, 100mg/L, 200mg/L, and 400mg/L, respectively.
CN202011512226.1A 2020-12-19 2020-12-19 Method for measuring components of oil and fat in cosmetics Active CN112684046B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011512226.1A CN112684046B (en) 2020-12-19 2020-12-19 Method for measuring components of oil and fat in cosmetics

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011512226.1A CN112684046B (en) 2020-12-19 2020-12-19 Method for measuring components of oil and fat in cosmetics

Publications (2)

Publication Number Publication Date
CN112684046A CN112684046A (en) 2021-04-20
CN112684046B true CN112684046B (en) 2023-02-10

Family

ID=75450395

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011512226.1A Active CN112684046B (en) 2020-12-19 2020-12-19 Method for measuring components of oil and fat in cosmetics

Country Status (1)

Country Link
CN (1) CN112684046B (en)

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2026746A2 (en) * 2006-05-31 2009-02-25 Ciba Holding Inc. Self tanning composition
CN101644697A (en) * 2009-06-10 2010-02-10 谱尼测试科技(北京)有限公司 Detection method of IPBC in cosmetics
CN104597166A (en) * 2015-02-09 2015-05-06 广西真龙实业有限责任公司 Method for detecting volatile organic compounds in cigarette tipping paper printing ink

Also Published As

Publication number Publication date
CN112684046A (en) 2021-04-20

Similar Documents

Publication Publication Date Title
CN106525997B (en) A method of organic acid and flavones ingredient in measurement serpentgrass
CN110824071B (en) Method for detecting lignans and flavonol glycosides in ginkgo leaf extract or preparation thereof
CN109655533A (en) A method of identifying flavors and fragrances type
CN112684050A (en) Research on determination method of whitening functional components in cosmetics
CN111413440A (en) Method for detecting parecoxib sodium sulfate genotoxic impurities
CN112034084A (en) Detection method of volatile components in blumea oil and application thereof
CN109187831B (en) Method for simultaneously and rapidly determining contents of 9 alcohol compounds in alcohol by adopting GC-MS (gas chromatography-Mass spectrometer)
CN112684046B (en) Method for measuring components of oil and fat in cosmetics
CN110133153A (en) Method that is a kind of while measuring 5 kinds of chemical composition contents in chrysanthemum medicinal material
CN113740448A (en) Olive oil flavor detection method based on electronic nose and gas phase-ion mobility spectrometry
CN107421975B (en) The detection method of glycerol content in a kind of injection
CN110333306B (en) Quantitative determination method for caprylic/capric glyceride in bead blasting solvent for cigarettes
CN110780002B (en) High-efficiency low-cost detection method for quantifying essential oil components
CN106706773A (en) GC-MS (gas chromatography-mass spectrometer) quantitative detection method for volatile components in cigarette glyceryl triacetate
CN114264752B (en) Detection method of methyl bromoacetate
CN110895264A (en) Method for determining ethyl bromide in tenofovir alafenamide
CN109613141A (en) The detection method of gamma lactone and delta-lactone class compound in a kind of quick-fried pearl liquid of cigarette filter tip
CN115078619A (en) GC-MS/MS method for simultaneously detecting 9N-nitrosamine impurities in valsartan preparation
CN108645932B (en) Method for rapidly screening prohibited essence and spice added in cream
CN102331463A (en) Method for measuring content of diethylene glycol in glyceryl triacetate
CN105974017B (en) The assay method of methanol content in flavouring essence for tobacco
CN104777260A (en) Brucea javanica oil emulsion injection liquid quality control method
CN116879428B (en) High performance liquid analysis method for residual content of phosphorylcholine in L-alpha-phosphorylcholine
CN115236239B (en) Method for detecting content of alpha-copaene in schisandra essential oil
CN113533607B (en) Method for evaluating quality of peony leaf medicinal material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant