CN106872608B - Method for simultaneously detecting 24 forbidden allergen essence substances in cosmetics - Google Patents
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Abstract
The invention relates to the technical field of compound detection, in particular to a method for detecting forbidden allergen essence substances in cosmetics. The detection method comprises the following steps: taking a cosmetic sample, and preparing a sample solution; detecting forbidden allergen essence substances in the sample solution by adopting a liquid chromatography-mass spectrometry analysis technology; the conditions of the liquid chromatography were: the chromatographic column is phenyl column, RP-MS or C18 chromatographic column; mobile phase a was acetonitrile and mobile phase B was 0.05% formic acid solution containing 5mM ammonium acetate; a gradient elution procedure; the conditions of mass spectrum are: an electrospray ion source; scanning positive ions; monitoring multiple reactions; the ion source temperature is 650 ℃; ion source voltage 5500V. The method has the advantages of low detection limit, high detection efficiency, good recovery rate and simultaneous qualitative and quantitative determination, and can be used for rapidly screening common perfume allergic chemical substances in cosmetics so as to meet the requirements of quality control and market supervision of enterprises at present and guarantee the safety of consumers.
Description
Technical Field
The invention relates to the technical field of compound detection, in particular to a detection method for simultaneously and rapidly detecting 24 forbidden allergen essence substances in cosmetics.
Background
With the continuous development of the reform and the openness of China, the economic level and the quality of life of people in China are continuously improved, the aesthetics is continuously changed, and cosmetics become a part of daily consumption of people and are also necessities of life. According to statistics, the annual sales of cosmetics in China in 2014 reaches 2000 billions, which accounts for about 8.8% of the global cosmetic market, and second to the United states, China becomes one of the largest global cosmetic markets. Statistically, an average of 12 personal care products per woman per day, containing 168 ingredients; on average, each male used 6 personal care products per day, containing 85 ingredients. Some of these ingredients can irritate the skin and cause allergic reactions. It is known that among complaints of cosmetics, complaints of skin allergy and adverse reactions occurring after the use of cosmetics usually account for 60 to 70% of the total complaints.
The cosmetic contains essence, antiseptic, excipient, surfactant, emulsifier, humectant, and natural components. At least 35% of cosmetic allergy is allergy caused by essence, which can cause skin allergy when directly contacting with skin, can cause human body allergy by breathing in the volatilization process, or causes skin allergy by photosensitization, and is a non-negligible allergen. The European Union of 2003 stipulates that 16 essence compounds including cinnamyl alcohol and the like are prohibited or limited from being used in cosmetics when the 76/768/EEC regulation is revised, and stipulates that 26 essences (2 of which are extracts) in daily essences from 3 months in 2005 must be indicated on the label of the cosmetic when the content is 0.001% or more in a non-washable type cosmetic and 0.01% or more in a washable type cosmetic.
At present, the detection of essence allergen substances in cosmetics mostly adopts gas chromatography, gas chromatography-mass spectrometry, liquid chromatography, gas chromatography-Fourier transform infrared spectroscopy combined (GC-FTIR) technology and the like. However, the methods have certain limitations because of complex cosmetic components, more aromatic and volatile substances, various dosage forms, complex types, more auxiliary agents and functional components such as an emulsifier, a lubricant, a surfactant and the like, high interference during gas chromatography or gas chromatography-mass spectrometry, high baseline, and analysis time of 30-40 minutes, and the problems of long analysis time, low peak separation degree and inaccurate qualification in liquid chromatography analysis.
Disclosure of Invention
In view of this, the invention provides a method for simultaneously and rapidly detecting 24 forbidden allergen perfume substances in cosmetics. The detection method has the advantages of small interference, low baseline, short analysis time, high separation degree and accurate qualitative and quantitative determination.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a detection method for simultaneously and rapidly detecting 24 forbidden allergen essence substances in cosmetics, which comprises the following steps:
taking a cosmetic sample, and preparing a sample solution;
detecting forbidden allergen essence substances in the sample solution by adopting a liquid chromatography-mass spectrometry analysis technology;
the conditions of the liquid chromatography were: the chromatographic column is phenyl column, RP-MS or C18 chromatographic column; mobile phase a was acetonitrile and mobile phase B was 0.05% formic acid solution containing 5mM ammonium acetate; a gradient elution procedure;
the conditions of mass spectrum are: electrospray ion source (ESI); scanning positive ions; multiple Reaction Monitoring (MRM); the ion source temperature is 650 ℃; ion source voltage 5500V;
the 24 contraindicated allergen fragrance materials include benzyl salicylate, α -isomethyl ionone, α -amyl cinnamaldehyde, β -citronellol, benzyl cinnamate, methyl 2-octynoate, α -amyl cinnamic alcohol, geraniol, benzyl alcohol, neocarvyl aldehyde, linalool, farnesol, cinnamic aldehyde, coumarin, α -hexyl cinnamic aldehyde, eugenol, benzyl benzoate, isoeugenol, lilac aldehyde, cinnamyl alcohol, anisyl alcohol, citral, α -carvylene, or hydroxycitronellaldehyde.
The liquid chromatogram-tandem mass spectrometry is a new technology developed in recent years, can obtain a strong quasi-molecular ion peak of an object to be detected under the condition of primary mass spectrometry, and can crack molecular ions by means of secondary mass spectrometry so as to obtain rich structural information. Compared with a gas chromatography method, a gas chromatography-mass spectrometry method, a liquid chromatography method and a gas chromatography-Fourier transform infrared spectroscopy (GC-FTIR) method, the technology has the characteristics of low detection limit, high sensitivity and strong anti-interference, aiming at 24 allergen substances in more cosmetic allergy cases reported at present, including benzyl salicylate, alpha-isomethylionone, alpha-amyl cinnamic aldehyde, beta-citronellol, benzyl cinnamate, 2-methyl octynoate, alpha-amyl cinnamic alcohol, geraniol, benzyl alcohol, lyral, linalool, farnesol, cinnamaldehyde, coumarin, alpha-hexyl cinnamic aldehyde, eugenol, benzyl benzoate, isoeugenol, lily of the valley aldehyde, cinnamyl alcohol, anisyl alcohol, citral, alpha-phellandrene, hydroxycitronellal and the like, the LC-MS/MS technology is firstly adopted, a high-flux and rapid screening method for simultaneously measuring 24 allergen essence substances in cosmetics is established, and rapid online qualitative and quantitative analysis can be carried out on common essence allergen chemical substances in cosmetics.
Preferably, the gradient elution procedure is: 0-6.0 min, 10-90% A; keeping 90% A for 6.0-8.0 min; 8.0-8.1 min, 90-10% A; keeping 10% A for 8.1-13.0 min.
Preferably, the flow rate of the liquid chromatography is 600. mu.L/min.
Preferably, the amount of sample to be applied by liquid chromatography is 10. mu.L.
Preferably, the parent ion, daughter ion, declustering voltage and collision energy parameters of the mass spectrum are as follows:
preferably, the atomizing gas, the gas curtain gas, the auxiliary gas and the collision gas under the mass spectrum condition are all high-purity nitrogen.
In the examples provided by the present invention, the cosmetic sample is a liquid sample or a cream, milky sample.
In one embodiment of the present invention, the cosmetic sample is a liquid sample, and the preparation method of the sample solution comprises: mixing cosmetic sample with acetonitrile and sodium chloride, ultrasonic extracting, and filtering.
In another embodiment of the present invention, the cosmetic sample is a cream or milky sample, and the preparation method of the sample solution comprises: mixing cosmetic sample with acetonitrile, ultrasonic extracting, adding sodium chloride, centrifuging, and filtering.
Preferably, the ratio of the cosmetic sample to the acetonitrile in g/mL is 2 (10-20).
In the examples provided herein, the ratio of cosmetic sample to acetonitrile in g/mL is 2: 10.
Preferably, the amount of sodium chloride added is such that a saturated solution of sodium chloride is formed.
Preferably, the ultrasonic extraction frequency is 28kHz, the temperature is 10-30 ℃, and the time is 15 min.
Preferably, the filtration is performed with a 0.22 μm membrane filter.
Preferably, the centrifugation is 9000r/min for 10 min.
The invention provides a detection method for simultaneously and rapidly detecting 24 forbidden allergen essence substances in cosmetics. The detection method comprises the following steps: taking a cosmetic sample, and preparing a sample solution; detecting forbidden allergen essence substances in the sample solution by adopting a liquid chromatography-mass spectrometry analysis technology; the conditions of the liquid chromatography were: the chromatographic column is phenyl column or C18 chromatographic column; mobile phase a was acetonitrile and mobile phase B was 0.05% formic acid solution containing 5mM ammonium acetate; a gradient elution procedure; the conditions of mass spectrum are: electrospray ion source (ESI); scanning positive ions; multiple Reaction Monitoring (MRM); the ion source temperature is 650 ℃; ion source voltage 5500V. The invention has at least one of the following advantages:
1. the invention establishes a liquid chromatography-tandem mass spectrometry rapid detection method for 24 forbidden allergic essence substances in different cosmetic matrixes. Aiming at the characteristics of complex substrate components, and many aromatic and volatile substances of the cosmetics, the invention adopts an LC-MS/MS technology to establish an on-line high-flux and rapid screening method capable of simultaneously and rapidly measuring 24 allergen essence substances in the cosmetics, and the detection limit of the method for various substrates of liquid and solid cosmetics can reach 5mg/kg, which is reduced by 50 percent compared with the method (10mg/kg) reported by the current domestic and foreign documents. The method has the advantages of low detection limit, high detection efficiency, good recovery rate and simultaneous qualitative and quantitative determination, and can be used for rapidly screening common perfume allergic chemical substances in cosmetics so as to meet the requirements of quality control and market supervision of enterprises at present and guarantee the safety of consumers.
2. LC-MS/MS is a tandem mass spectrum, compounds are characterized by cracking an excimer ion peak into a daughter ion, and the compounds can be combined with retention time for characterization, so that the characterization is more accurate than GC-MS, GC and LC.
3. The instrument analysis time of each sample in the method is 13min, while the analysis method time reported in the current similar documents is respectively 30 minutes and 40 minutes which is 2.3-3.1 times of that of the method.
4. When the liquid chromatography-tandem mass spectrometry is adopted, due to the fact that different compound cracking modes and cracking ion pairs are different, proper ion pairs can be selected according to factors such as the peak emergence time of different compounds, background interference, interference of other compounds and the like, so that the ion pairs are separated on an extracted ion pair diagram, and the problem of inaccurate quantification caused by poor peak separation degree in detection of gas chromatography and liquid chromatography is solved.
5. The cosmetic contains surfactant, and the water removing agent sodium chloride has salting-out effect, and can effectively improve the condition of non-ideal demulsification when anhydrous sodium sulfate is used in literature method.
6. Aiming at the matrix characteristics of cosmetics, the universal pretreatment methods of different cosmetic matrixes are determined, including the universal pretreatment methods of matrixes such as cream, water, emulsion and the like, so that the sample is purified to the maximum extent, and the good recovery rate of the target compound is ensured.
Drawings
FIG. 1 shows a total ion flow diagram of 24 allergen fragrance materials in a toner standard add-on sample; 1 is anisyl alcohol; 2-7 are limonene, linalool, hydroxycitronellal, cinnamyl alcohol, cinnamyl aldehyde and geraniol respectively; 8 is eugenol; 9 is isoeugenol; 10 is lyral; 11 is amyl cinnamic alcohol; 12 is coumarin; 13 is farnesol; 14 is citral; 15 is octynoic acid methyl ester; 16 is benzyl benzoate; 17 is rhodinol; 18 is benzyl cinnamate; 19 is benzyl salicylate; 20 is ionone; 21 is amyl cinnamaldehyde; 22 is hexyl cinnamic aldehyde; 23 is lilial; 24 is benzyl alcohol;
FIG. 2 shows a quantitative ion pair extraction diagram of a toner standard addition sample;
FIG. 3 shows secondary mass spectra of 24 compounds;
FIG. 4 shows a toner negative matrix total ion flow graph.
Detailed Description
The invention discloses a method for simultaneously and rapidly detecting 24 forbidden allergen essence substances in cosmetics, and a person skilled in the art can use the contents for reference and appropriately improve process parameters to realize the detection. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The reagent or instrument used in the method for detecting the forbidden allergen essence substances in the cosmetics can be purchased from the market.
The invention is further illustrated by the following examples:
example 1
1. The pretreatment method comprises the following steps:
(1) liquid sample: accurately weighing 2.0g of sample into a 10mL colorimetric tube with a plug, accurately adding 10mL of acetonitrile and a proper amount of sodium chloride (until the sodium chloride is separated out), uniformly mixing by vortex, ultrasonically extracting for 15min, filtering by a 0.22 mu m filter membrane, and loading on a machine.
(2) Paste, milky sample: accurately weighing 2.0g of sample in a 50mL centrifuge tube, accurately adding 10mL acetonitrile, vortex and mixing uniformly, carrying out ultrasonic extraction for 15min, adding a proper amount of sodium chloride (until the sodium chloride is separated out), centrifuging at 9000r/min for 10min, filtering through a 0.22 mu m filter membrane, loading on a machine, and carrying out external standard method quantification.
2. Chromatographic conditions are as follows:
the chromatographic column is phenyl column, RP-MS or C18 chromatographic column;
mobile phase: a is acetonitrile and B is 0.05% formic acid solution (containing 5mM ammonium acetate).
Gradient elution procedure: 0-6.0 min, 10-90% A; keeping 90% A for 6.0-8.0 min; 8.0-8.1 min, 90-10% A; keeping 10% A for 8.1-13.0 min.
The flow rate was 600. mu.L/min and the amount of sample was 10. mu.L.
3. Mass spectrum conditions:
electrospray ion source (ESI); scanning positive ions; multiple Reaction Monitoring (MRM); the ion source temperature is 650 ℃; ion source voltage 5500V; the atomizing gas, the gas curtain gas, the auxiliary gas and the collision gas are all high-purity nitrogen. MRM monitors ion pairs, declustering voltage and collision voltage as follows:
mass spectrum optimization conditions of 124 essence allergen compounds in table
Test example 1
1. The pretreatment method comprises the following steps:
liquid sample: accurately weighing 2.0g of toner standard addition sample in a 10mL colorimetric tube with a plug, accurately adding 10mL of acetonitrile and a proper amount of sodium chloride (until the sodium chloride is separated out), vortex mixing, ultrasonically extracting for 15min, filtering with a 0.22 μm filter membrane, and packaging.
2. Chromatographic conditions are as follows:
the column is a phenyl column, an Accucore Ph/Hex column (150 mm. times.3.0 mm i.d., 2.6 μm);
mobile phase: a is acetonitrile and B is 0.05% formic acid solution (containing 5mM ammonium acetate).
Gradient elution procedure: 0-6.0 min, 10-90% A; keeping 90% A for 6.0-8.0 min; 8.0-8.1 min, 90-10% A; keeping 10% A for 8.1-13.0 min.
The flow rate was 600. mu.L/min and the amount of sample was 10. mu.L.
3. Mass spectrum conditions:
electrospray ion source (ESI); scanning positive ions; multiple Reaction Monitoring (MRM); the ion source temperature is 650 ℃; ion source voltage 5500V; the atomizing gas, the gas curtain gas, the auxiliary gas and the collision gas are all high-purity nitrogen. MRM monitors ion pairs, declustering voltage and collision voltage as shown in table 1.
The total ion flow chart of 24 allergen essence substances in the toner standard addition sample is shown in figure 1, the quantitative ion pair extraction chart is shown in figure 2, and the secondary mass spectrogram of 24 compounds is shown in figure 3.
As can be seen from FIG. 2, the method of the present invention employs liquid chromatography-tandem mass spectrometry detection, and the selected ion pairs are suitable, and the individual compounds can be well separated on the extracted ion pair graph.
The total ion flow chart of the toner negative matrix is shown in figure 4, and the comparison between figure 1 and figure 4 shows that the pretreatment method and the instrument method of the invention have no background interference in the sample and satisfactory purification effect.
Test example 2
1. The pretreatment method comprises the following steps:
paste, milky sample: accurately weighing 2.0g of sample in a 50mL centrifuge tube, accurately adding 10mL acetonitrile, vortex and mixing uniformly, carrying out ultrasonic extraction for 15min, adding a proper amount of sodium chloride (until the sodium chloride is separated out), centrifuging at 9000r/min for 10min, filtering through a 0.22 mu m filter membrane, loading on a machine, and carrying out external standard method quantification.
2. Chromatographic conditions are as follows:
the chromatographic column is a C18 chromatographic column, an Accucore C18 chromatographic column (150mm × 3.0mm i.d., 2.6 μm);
mobile phase: a is acetonitrile and B is 0.05% formic acid solution (containing 5mM ammonium acetate).
Gradient elution procedure: 0-6.0 min, 10-90% A; keeping 90% A for 6.0-8.0 min; 8.0-8.1 min, 90-10% A; keeping 10% A for 8.1-13.0 min.
The flow rate was 600. mu.L/min and the amount of sample was 10. mu.L.
3. Mass spectrum conditions:
electrospray ion source (ESI); scanning positive ions; multiple Reaction Monitoring (MRM); the ion source temperature is 650 ℃; ion source voltage 5500V; the atomizing gas, the gas curtain gas, the auxiliary gas and the collision gas are all high-purity nitrogen. MRM monitors ion pairs, declustering voltage and collision voltage as shown in table 1.
The detection result is similar to that of the test example 1, and the 24 compounds can be separated without background interference.
Test example 3
Selection of chromatographic column: through experimental investigation, the target compound has good response and peak shape on a phenyl column, an RP-MS or a C18 chromatographic column;
the linear relationship, detection limit, recovery rate and precision of the detection method of test example 1 were examined, and the test results were as follows:
1. linear relationship and detection limit: the peak areas Y of the target compounds are respectively used as vertical coordinates, the corresponding concentration values X are used as horizontal coordinates, and standard curves are drawn, so that the results show that the concentrations and the peak areas of the 24 target compounds are in good linear relation within the range of 1.0-5.0 mu g/mL. The linear equation and the correlation coefficient are shown in the following table:
linear equation and related coefficient of 224 flavor and fragrance allergen substances in table
At the signal-to-noise ratio (R) of actual detectionS/N) The detection limit is 3, the instrument detection limit is 1.0 mug/mL, the method detection limit of various cosmetic matrixes is 10mg/kg, and the quantitative limit is 30 mg/kg.
2. Recovery and precision: the recovery rate and precision of 24 forbidden allergen essence substances in the toner are inspected by adopting a negative sample standard addition method, and experimental data are shown in the following table:
table 3 mean recovery and relative standard deviation of the target compound at 3 added levels in toner (n ═ 10)
As can be seen from the above table, the recovery rate after the toner negative sample standard is added ranges from 85.9% to 110%, and the precision is between 5.5% to 12%, thus meeting the requirements of SN/T4537-.
Comparative example 1
The retention time of the target compound benzyl cinnamate which finally appears in a peak in a literature method, namely gas chromatography-mass spectrometry determination of 24 allergens in cosmetics, is 30.49 minutes, while the retention time of the target compound benzyl alcohol which finally appears in the method is 7.12 minutes, so that the analysis time is greatly shortened.
Comparative example 2
In the literature method, in C.Villa and the like in a High-performance liquid chromatographic method for the simultaneous determination of 24 types of forbidden perfume components, 24 types of forbidden perfume components are simultaneously determined by using a High performance liquid chromatography (DAD detector) and a C18 chromatographic column, and the analysis time of each sample instrument is 40min, but many chromatographic peaks are still not well separated, and the quantitative accuracy is not High.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method for detecting forbidden allergen perfume substances in cosmetics is characterized by comprising the following steps:
taking a cosmetic sample, and preparing a sample solution;
simultaneously detecting forbidden allergen essence substances in the sample solution by adopting a liquid chromatography-mass spectrometry analysis technology;
the conditions of the liquid chromatography are as follows: the chromatographic column is phenyl column or C18 chromatographic column; the specification of the chromatographic column is 150mm multiplied by 3.0mm i.d., 2.6 μm; mobile phase a was acetonitrile and mobile phase B was 0.05% formic acid solution containing 5mM ammonium acetate; a gradient elution procedure;
the mass spectrum conditions are as follows: an electrospray ion source; scanning positive ions; monitoring multiple reactions; the ion source temperature is 650 ℃; ion source voltage 5500V;
the forbidden allergen essence substances are benzyl salicylate, alpha-isomethyl ionone, alpha-amyl cinnamic aldehyde, beta-citronellol, benzyl cinnamate, methyl 2-octynoate, alpha-amyl cinnamic alcohol, geraniol, benzyl alcohol, lyral, linalool, farnesol, cinnamic aldehyde, coumarin, alpha-hexyl cinnamic aldehyde, eugenol, benzyl benzoate, isoeugenol, lilac aldehyde, cinnamyl alcohol, anisic alcohol, citral, alpha-carveene and hydroxycitronellal;
the gradient elution procedure was: 0-6.0 min, 10% A-90% A; keeping 90% A for 6.0-8.0 min; 8.0-8.1 min, 90-10% A; keeping 10% A for 8.1-13.0 min;
the parent ion, the daughter ion, the declustering voltage and the collision energy parameters of the mass spectrum are as follows:
。
2. The detection method according to claim 1, wherein the flow rate of the liquid chromatography is 600 μ L/min.
3. The detection method according to claim 1, wherein the liquid chromatography is carried out in an amount of 10 μ L.
4. The detection method according to any one of claims 1 to 3, wherein the atomizing gas, the curtain gas, the assist gas and the collision gas of the mass spectrometry condition are all high-purity nitrogen gas.
5. The detection method according to claim 1, wherein the cosmetic sample is a liquid sample or a paste-like, milky sample.
6. The detection method according to claim 5, wherein the cosmetic sample is a liquid sample, and the sample solution is prepared by: mixing cosmetic sample with acetonitrile and sodium chloride, ultrasonic extracting, and filtering.
7. The detection method according to claim 5, wherein the cosmetic sample is a cream or milky sample, and the sample solution is prepared by: mixing cosmetic sample with acetonitrile, ultrasonic extracting, adding sodium chloride, centrifuging, and filtering.
8. The detection method according to claim 6 or 7, wherein the ratio of the cosmetic sample to acetonitrile in g/mL is 2 (10-20).
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| CN108828102B (en) * | 2018-08-20 | 2020-11-03 | 云南同创检测技术股份有限公司 | Method for determining content of pineapple ester and jasmal in essence and flavor |
| CN109884216A (en) * | 2019-04-10 | 2019-06-14 | 西南医科大学 | A kind of method that high performance liquid chromatography measures method Buddhist nun's aldehyde in carrier micelle |
| CN110174488B (en) * | 2019-06-10 | 2021-08-24 | 青岛农业大学 | Method for detecting allergen in cosmetics |
| CN111122747A (en) * | 2019-12-31 | 2020-05-08 | 汕头出入境检验检疫局检验检疫技术中心 | Method for analyzing sensitized aromatic substances in cosmetics |
| CN114924013A (en) * | 2022-05-12 | 2022-08-19 | 广东铭康香精香料有限公司 | Method for determining various perfume ingredients in cosmetics by gas chromatography-tandem mass spectrometry |
| CN115032312B (en) * | 2022-07-15 | 2023-10-03 | 浙江省产品质量安全科学研究院 | Method for simultaneously detecting multiple sensitization fragrances in mosquito-repellent product |
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