CN106872608A - Limited in a kind of cosmetics with the detection method of anaphylactogen perfume materials - Google Patents
Limited in a kind of cosmetics with the detection method of anaphylactogen perfume materials Download PDFInfo
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Abstract
The present invention relates to compound test technical field, limited in more particularly to a kind of cosmetics with the detection method of anaphylactogen perfume materials.The detection method includes：Cosmetic sample is taken, sample solution is prepared；Anaphylactogen perfume materials are used using being limited in LC Mass technology for detection sample solution；The condition of liquid chromatogram is：Chromatographic column is phenyl post, RP MS or C18 chromatographic columns；Mobile phase A is acetonitrile, and Mobile phase B is 0.05% formic acid solution containing 5mM ammonium acetates；Gradient elution program；Mass spectrographic condition is：Electric spray ion source；Cation is scanned；Multiple-reaction monitoring；650 DEG C of ion source temperature；Ion source voltage 5500V.The method has the advantages that test limit is low, detection efficiency is high, the rate of recovery good, can qualitative, quantitative simultaneously, can be used for the rapid screening of common spices anaphylaxis chemical substance in cosmetics, with the demand for meeting current enterprise's Quality Control, market surpervision and ensureing consumer safety.
Description
Technical field
The present invention relates to compound test technical field, limited in more particularly to a kind of cosmetics and use anaphylactogen perfume materials
Detection method.
Background technology
With continuing to develop that China reforms and opens up to the outside world, our people's economic level is also being improved constantly with quality of life, is examined
Attractive in appearance to be continually changing, cosmetics become a part for people's current consumption, are also daily necessities.According to statistics, 2014 I
State's cosmetics annual sales amount accounts for the 8.8% of global Cosmetic Market up to more than 2,000 hundred million yuan, is only second to the U.S., and China has turned into
One of global maximum Cosmetic Market.According to statistics, average every women uses 12 kinds of personal care articles daily, comprising 168 kinds into
Point；Average every male uses 6 kinds of personal care articles daily, comprising 85 kinds of compositions.Some materials can stimulate skin in these compositions
Skin and cause allergic reaction.It is reported that, it is allergic and adverse reaction using occurring after cosmetics in toiletries complaint
Complaint is typically constituted complains 60% to the 70% of total amount.
In cosmetics sensitizer have essence, preservative, excipient, surfactant, emulsifying agent, NMF, it is natural into
Grade.At least 35% is the allergy caused by essence wherein in cosmetic allergic contact dermatitis, and it can cause when with direct skin contact
It is allergic, also human allergy can be caused by breathing in its volatilization process, or caused by photosensitization it is allergic,
It is very important anaphylactogen.European Union in 2003 regulation, 16 kinds of essence such as including cinnamyl alcohol when 76/768/EEC regulations are revised
Compound be inhibited in cosmetics using or limitation use, and specify from March, 2005 26 kinds of essence (its in daily essence
In 2 kinds be extract) content is more than or equal to 0.001%, contains in flushable type cosmetics such as in not flushable type cosmetics
When amount is more than or equal to 0.01%, it is necessary to indicated on the cosmetics label.
At present to more than the detection of essence class allergenic agent in cosmetics using gas chromatography, gas chromatography-mass spectrography,
Liquid chromatography, gas-chromatography-FFIR combination (GC-FTIR) technology etc..But because cosmetic composition is multiple
Miscellaneous, armaticity, volatile materials are more, and formulation is various, broad categories, and the auxiliary agent such as emulsifying agent, lubricant, surfactant,
Functional components are more, disturb larger when gas-chromatography or gas chromatography-mass spectrography, and baseline is higher, analysis time be 30~
40 minutes, and liquid-phase chromatographic analysis there is also that analysis time is long, peak separating degree is not high, can not accurate qualitatively problem, therefore this
A little methods are respectively provided with certain limitation.
The content of the invention
In view of this, the invention provides the detection method that use anaphylactogen perfume materials are limited in a kind of cosmetics.The inspection
The interference of survey method is small, and baseline is low, and analysis time is short, and separating degree is high, can be accurately qualitative, quantitative.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides being limited in a kind of cosmetics with the detection method of anaphylactogen perfume materials, comprise the following steps：
Cosmetic sample is taken, sample solution is prepared；
Anaphylactogen perfume materials are used using being limited in LC-MS analysis technology for detection sample solution；
The condition of liquid chromatogram is：Chromatographic column is phenyl post, RP-MS or C18 chromatographic columns；Mobile phase A is acetonitrile, mobile phase
B is 0.05% formic acid solution containing 5mM ammonium acetates；Gradient elution program；
Mass spectrographic condition is：Electric spray ion source (ESI)；Cation is scanned；Multiple-reaction monitoring (MRM)；Ion source temperature
650℃；Ion source voltage 5500V；
Limit and be selected from benzyl salicylate, α-daphnone, jasminal, β-perfume with anaphylactogen perfume materials
Thatch alcohol, benzyl cinnamate, methyl 2-octynoate, α amylcinnamic alcohol, geraniol, phenmethylol, lyral, linalool, Jin He
Joyous alcohol, cinnamic acid, cumarin, jasmonal H, eugenol, Benzyl Benzoate base ester, isoeugenol, lilial, cinnamyl alcohol, fennel
Aromatic, citral, α-carvene or laurine.
Liquid Chromatography-Tandem Mass Spectrometry is a kind of new technology that developed recently gets up, and can be obtained under the conditions of first mass spectrometric
Very strong determinand quasi-molecular ion peak, and quasi-molecular ion can be cracked by second order mses, and then enriched
Structural information.The technology becomes than gas chromatography, gas chromatography-mass spectrography, liquid chromatography, gas-chromatography-Fourier
Change infrared spectrum combination (GC-FTIR) method and have that test limit is low, sensitivity is high, it is anti-interference strong the characteristics of, the present invention is for current
24 kinds of allergenic agents in the more cosmetic allergic contact dermatitis case of report, including benzyl salicylate, α-daphnone, α-
Amyl cinnamic aldehyde, β-citronellol, benzyl cinnamate, methyl 2-octynoate, α amylcinnamic alcohol, geraniol, phenmethylol, the new lily of the valley
Aldehyde, linalool, fanesol, cinnamic acid, cumarin, jasmonal H, eugenol, Benzyl Benzoate base ester, isoeugenol, bell
Blue aldehyde, cinnamyl alcohol, anise alcohol, citral, α-carvene, laurine etc., first using LC-MS/MS technologies, establishing
The 24 kinds of high fluxs of anaphylactogen perfume materials, quick screening methods in cosmetic, can be to common essence anaphylactogen chemistry in cosmetics
Material carries out quick online qualitative and quantitative analysis.
Preferably, gradient elution program is：0~6.0min, 10%A~90%A；6.0~8.0min, keeps 90%A；
8.0~8.1min, 90%A~10%A；8.1~13.0min, keeps 10%A.
Preferably, the μ L/min of flow velocity 600 of liquid chromatogram.
Preferably, the sample size of liquid chromatogram is 10 μ L.
Preferably, mass spectrographic parent ion, daughter ion, going cluster voltage and collision energy parameter as follows：
Preferably, the atomization gas of Mass Spectrometry Conditions, gas curtain gas, auxiliary gas and collision gas are high pure nitrogen.
In the embodiment that the present invention is provided, cosmetic sample is liquid sample or paste, emulsus sample.
In the specific embodiment that the present invention is provided, cosmetic sample is liquid sample, the preparation side of its sample solution
Method is：Cosmetic sample is mixed with acetonitrile, sodium chloride, ultrasonic extraction, filtered.
The present invention provide another specific embodiment in, cosmetic sample be paste, emulsus sample, its sample solution
Preparation method is：Cosmetic sample is mixed with acetonitrile, ultrasonic extraction, add sodium chloride, centrifugation, filtering.
Preferably, in terms of g/mL, the ratio of cosmetic sample and acetonitrile is 2:(10~20).
In the embodiment that the present invention is provided, in terms of g/mL, the ratio of cosmetic sample and acetonitrile is 2:10.
Preferably, the addition of sodium chloride is the amount to form sodium chloride saturated solution.
Preferably, the frequency of ultrasonic extraction is 28kHz, temperature is 10~30 DEG C, and the time is 15min.
Preferably, being filtered into using 0.22 μm of membrane filtration.
Preferably, centrifugation is centrifuged 10min for 9000r/min.
The invention provides the detection method that use anaphylactogen perfume materials are limited in a kind of cosmetics.The detection method bag
Include：Cosmetic sample is taken, sample solution is prepared；It is used using being limited in LC-MS analysis technology for detection sample solution
Quick former perfume materials；The condition of liquid chromatogram is：Chromatographic column is phenyl post or C18 chromatographic columns；Mobile phase A is acetonitrile, Mobile phase B
It is 0.05% formic acid solution containing 5mM ammonium acetates；Gradient elution program；Mass spectrographic condition is：Electric spray ion source (ESI)；Just
Ion scan；Multiple-reaction monitoring (MRM)；650 DEG C of ion source temperature；Ion source voltage 5500V.The present invention at least has following excellent
One of gesture：
1st, the present invention establish a kind of 24 kinds limit with anaphylaxis perfume materials in different cosmetic bases liquid chromatogram-
Tandem mass spectrum detection method.The present invention is directed to cosmetic base complicated component, armaticity, the characteristics of volatile materials is more, uses
LC-MS/MS technologies, setting up can the 24 kinds of online high fluxs of anaphylactogen perfume materials, quick sieve in Rapid Simultaneous Determination cosmetics
The method test limit of checking method, liquid and the various matrix of solid, cosmetic is reported up to 5mg/kg than current domestic and foreign literature
Method (10mg/kg), reduce 50%.The method has that test limit is low, detection efficiency is high, the rate of recovery good, can be simultaneously qualitative
Quantitative advantage, can be used for the rapid screening of common spices anaphylaxis chemical substance in cosmetics, with meet current enterprise's Quality Control,
Market surpervision and the demand of guarantee consumer safety.
2nd, LC-MS/MS be tandem mass spectrometry, daughter ion is cracked into by quasi-molecular ion peak, compound is carried out it is qualitative, and
Retention time can be combined qualitative therefore qualitative than GC-MS and GC, LC more accurate.
3rd, the Instrumental Analysis time of each sample of the inventive method is 13min, and the analysis side of close document report at present
The method time is respectively more than 30 minutes and 40 minutes, is 2.3~3.1 times of this method.
When the 4th, using liquid chromatography-tandem mass spectrometry, because different compound cracking modes and cracking ion pair are variant, can
The factors such as appearance time, ambient interferences, other compounds interference according to different compounds, select suitable ion pair, so that
Separated on ion pair figure is extracted, peak separating degree is bad during solving gas-chromatography, liquid chromatographic detection and then causes to determine
The inaccurate problem of amount.
5th, surfactant is contained in cosmetics, the dehydration reagent sodium chloride that the method is added has salting out concurrently, can be effective
Be demulsified undesirable situation when improving literature method using anhydrous sodium sulfate.
6th, for the matrix feature of cosmetics, determine the general pre-treating method of different cosmetic bases, including cream, frost,
The general pre-treating method of the matrix such as water, emulsion, carries out purified treatment, and ensure that target compound is good to sample to greatest extent
The good rate of recovery.
Brief description of the drawings
Fig. 1 shows 24 kinds of total ion current figures of anaphylactogen perfume materials in skin toner water quality standard addition sample；1 is anisyl alcohol；
2-7 is respectively limonene, linalool, laurine, cinnamyl alcohol, cinnamic acid, geraniol；8 is eugenol；9 is isoeugenol；
10 is lyral；11 is amyl group cinnamyl alcohol；12 is cumarin；13 is fanesol；14 is citral；15 is octynic acid first
Ester；16 is Ergol；17 is rhodinol；18 is benzyl cinnamate；19 is benzyl salicylate；20 is irisone；21 are
Amyl cinnamic aldehyde；22 is jasminolene；23 is lilial；24 is phenmethylol；
Fig. 2 shows that skin toner water quality standard adds sample amounts ion pair extraction figure；
Fig. 3 shows 24 kinds of second order mses figures of compound；
Fig. 4 shows toner anima total ion current figure.
Specific embodiment
The invention discloses the detection method that use anaphylactogen perfume materials are limited in a kind of cosmetics, those skilled in the art
Present disclosure can be used for reference, technological parameter realization is suitably modified.In particular, all similar replacements and change are right
It is it will be apparent that they are considered as being included in the present invention for those skilled in the art.The method of the present invention and application are
It is described through by preferred embodiment, related personnel can be not substantially being departed from present invention, spirit and scope to this
Methods and applications described in text are modified or suitably change is realized and apply the technology of the present invention with combining.
Limited in the cosmetics that the present invention is provided equal with agents useful for same in the detection method of anaphylactogen perfume materials or instrument
Can be bought by market.
With reference to embodiment, the present invention is expanded on further：
Embodiment 1
1st, pre-treating method：
(1) liquid sample：It is accurate to weigh sample 2.0g in 10mL color-comparison tubes, the accurate 10mL acetonitriles and appropriate of adding
Sodium chloride (is separated out) to sodium chloride, is vortexed and is mixed, and ultrasonic extraction 15min crosses 0.22 μm of membrane filtration, upper machine.
(2) paste, emulsus sample：Accurate to weigh sample 2.0g in 50mL centrifuge tubes, accurate addition 10mL acetonitriles are vortexed
Mix, ultrasonic extraction 15min, plus appropriate sodium chloride (being separated out to sodium chloride), 9000r/min centrifugation 10min, cross 0.22 μm of filter membrane
Filtering, upper machine, quantified by external standard method.
2nd, chromatographic condition：
Chromatographic column is phenyl post, RP-MS or C18 chromatographic columns；
Mobile phase：A is acetonitrile, and B is 0.05% formic acid solution (ammonium acetate containing 5mM).
Gradient elution program：0~6.0min, 10%A~90%A；6.0~8.0min, keeps 90%A；8.0~
8.1min, 90%A~10%A；8.1~13.0min, keeps 10%A.
The μ L/min of flow velocity 600, sample size is 10 μ L.
3rd, Mass Spectrometry Conditions：
Electric spray ion source (ESI)；Cation is scanned；Multiple-reaction monitoring (MRM)；650 DEG C of ion source temperature；Ion gun electricity
Pressure 5500V；Atomization gas, gas curtain gas, auxiliary gas and collision gas are high pure nitrogen.MRM monitors ion pair, goes cluster voltage and collision
Voltage see the table below：
1 24 kinds of mass spectrum optimal conditions of essence anaphylactogen compound of table
Test example 1
1st, pre-treating method：
Liquid sample：The accurate skin toner water quality standard that weighs adds sample 2.0g in 10mL color-comparison tubes, accurately adds
10mL acetonitriles and appropriate sodium chloride (being separated out to sodium chloride), are vortexed and mix, and ultrasonic extraction 15min crosses 0.22 μm of membrane filtration, on
Machine.
2nd, chromatographic condition：
Chromatographic column is phenyl post, Accucore Ph/Hex chromatographic columns (150mm × 3.0mm i.d., 2.6 μm)；
Mobile phase：A is acetonitrile, and B is 0.05% formic acid solution (ammonium acetate containing 5mM).
Gradient elution program：0~6.0min, 10%A~90%A；6.0~8.0min, keeps 90%A；8.0~
8.1min, 90%A~10%A；8.1~13.0min, keeps 10%A.
The μ L/min of flow velocity 600, sample size is 10 μ L.
3rd, Mass Spectrometry Conditions：
Electric spray ion source (ESI)；Cation is scanned；Multiple-reaction monitoring (MRM)；650 DEG C of ion source temperature；Ion gun electricity
Pressure 5500V；Atomization gas, gas curtain gas, auxiliary gas and collision gas are high pure nitrogen.MRM monitors ion pair, goes cluster voltage and collision
Voltage is shown in Table 1.
The total ion current figure of 24 kinds of anaphylactogen perfume materials is shown in Fig. 1 in skin toner water quality standard addition sample, and quota ion pair is carried
Take figure and see Fig. 2, the second order mses figure of 24 kinds of compounds is shown in Fig. 3.
From Figure 2 it can be seen that the inventive method is detected using liquid chromatography-tandem mass spectrometry, selected ion pair is suitable, extract from
Son on figure to that well can separate each compound.
Toner anima total ion current figure is shown in Fig. 4, Fig. 1 is compared with Fig. 4 and is understood afterwards, by pre-treatment of the invention
Method and instrumental method, without ambient interferences in sample, clean-up effect satisfaction.
Test example 2
1st, pre-treating method：
Paste, emulsus sample：Accurate to weigh sample 2.0g in 50mL centrifuge tubes, accurate to add 10mL acetonitriles, vortex is mixed
It is even, ultrasonic extraction 15min, plus appropriate sodium chloride (being separated out to sodium chloride), 9000r/min centrifugation 10min, cross 0.22 μm of filter membrane mistake
Filter, upper machine, quantified by external standard method.
2nd, chromatographic condition：
Chromatographic column is C18 chromatographic columns, Accucore C18 chromatographic columns (150mm × 3.0mm i.d., 2.6 μm)；
Mobile phase：A is acetonitrile, and B is 0.05% formic acid solution (ammonium acetate containing 5mM).
Gradient elution program：0~6.0min, 10%A~90%A；6.0~8.0min, keeps 90%A；8.0~
8.1min, 90%A~10%A；8.1~13.0min, keeps 10%A.
The μ L/min of flow velocity 600, sample size is 10 μ L.
3rd, Mass Spectrometry Conditions：
Electric spray ion source (ESI)；Cation is scanned；Multiple-reaction monitoring (MRM)；650 DEG C of ion source temperature；Ion gun electricity
Pressure 5500V；Atomization gas, gas curtain gas, auxiliary gas and collision gas are high pure nitrogen.MRM monitors ion pair, goes cluster voltage and collision
Voltage is shown in Table 1.
Its testing result is close with test example 1, can equally separate 24 kinds of compounds, and without ambient interferences.
Test example 3
The selection of chromatographic column：Found through experiment investigation, target compound is respectively provided with phenyl post, RP-MS or C18 chromatographic columns
Good response and peak shape；
Linear relationship, detection limit, the rate of recovery and the precision of the detection method of test example 1 are investigated, result of the test is as follows：
1st, linear relationship and detection limit：The peak area Y with target compound is as ordinate respectively, with corresponding concentration value X
It is abscissa, makees standard curve, as a result shows, 24 kinds of target compounds concentration and peak area in the range of 1.0~5.0 μ g/mL
It is in good linear relationship.Linear equation and coefficient correlation see the table below：
The linear equation and coefficient correlation of 2 24 kinds of essence and flavoring agent class allergenic agents of table
With it is actually detected when signal to noise ratio (RS/N) for 3 used as detection limit, instrument detection limit is 1.0 μ g/mL, and cosmetics are each
The method detection for planting matrix is limited to 10mg/kg, is quantitatively limited to 30mg/kg.
2nd, the rate of recovery and precision：24 kinds in toner are limited using negative sample standard addition method uses anaphylactogen essence
Material has carried out the rate of recovery and precision is investigated, and experimental data see the table below：
The average recovery rate of target compound and relative standard deviation (n=10) under 3 pitch-based spheres in the toner of table 3
As seen from the above table, rate of recovery scope is accurate between 85.9%~110% after the addition of toner negative sample standard
Degree meets SN/T 4537-2016 between 5.5%~12%《Import and export food, cosmetics detection quality control guide (are changed
Learn)》It is required that.
Comparative example 1
Literature method《24 kinds of Gas Chromatography-Mass Spectrometries of anaphylactogen in cosmetics》In last appearance target chemical combination
Thing benzyl cinnamate retention time be 30.49 minutes, and in this method last appearance target compound phenmethylol retention time
It it is 7.12 minutes, analysis time greatly shortens.
Comparative example 2
Literature method《High-performance liquid chromatographic method for the
simultaneous determination of 24 fragrance allergens to study scented
products》Middle C.Villa etc. determines 24 kinds of disablings simultaneously using high performance liquid chromatography (DAD detectors), C18 chromatographic columns
Fragrance component, each sample instrument analysis time is 40min, but many chromatographic peaks are still without preferably being separated, quantitative standard
True property is not high.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. limited in a kind of cosmetics with the detection method of anaphylactogen perfume materials, it is characterised in that comprise the following steps：
Cosmetic sample is taken, sample solution is prepared；
Anaphylactogen perfume materials are used using being limited in sample solution described in LC-MS analysis technology for detection；
The condition of the liquid chromatogram is：Chromatographic column is phenyl post, RP-MS or C18 chromatographic columns；Mobile phase A is acetonitrile, mobile phase
B is 0.05% formic acid solution containing 5mM ammonium acetates；Gradient elution program；
The mass spectrographic condition is：Electric spray ion source；Cation is scanned；Multiple-reaction monitoring；650 DEG C of ion source temperature；Ion
Source voltage 5500V；
Described limiting is selected from benzyl salicylate, α-daphnone, jasminal, β-perfume with anaphylactogen perfume materials
Thatch alcohol, benzyl cinnamate, methyl 2-octynoate, α amylcinnamic alcohol, geraniol, phenmethylol, lyral, linalool, Jin He
Joyous alcohol, cinnamic acid, cumarin, jasmonal H, eugenol, Benzyl Benzoate base ester, isoeugenol, lilial, cinnamyl alcohol, fennel
Aromatic, citral, α-carvene or laurine.
2. detection method according to claim 1, it is characterised in that the gradient elution program is：0~6.0min,
10%A~90%A；6.0~8.0min, keeps 90%A；8.0~8.1min, 90%A~10%A；8.1~13.0min, keeps
10%A.
3. detection method according to claim 1 and 2, it is characterised in that the μ L/min of flow velocity 600 of the liquid chromatogram.
4. detection method according to any one of claim 1 to 3, it is characterised in that the sample size of the liquid chromatogram
It is 10 μ L.
5. detection method according to any one of claim 1 to 4, it is characterised in that the mass spectrographic parent ion, son from
Son, go cluster voltage and collision energy parameter as follows：
6. detection method according to any one of claim 1 to 5, it is characterised in that the atomization gas of the Mass Spectrometry Conditions,
Gas curtain gas, auxiliary gas and collision gas are high pure nitrogen.
7. detection method according to any one of claim 1 to 6, it is characterised in that the cosmetic sample is liquid
Sample or paste, emulsus sample.
8. detection method according to any one of claim 1 to 7, it is characterised in that the cosmetic sample is liquid
Sample, the preparation method of its sample solution is：Cosmetic sample is mixed with acetonitrile, sodium chloride, ultrasonic extraction, filtered.
9. detection method according to any one of claim 1 to 8, it is characterised in that the cosmetic sample be paste,
Emulsus sample, the preparation method of its sample solution is：Cosmetic sample is mixed with acetonitrile, ultrasonic extraction, add sodium chloride, from
The heart, filtering.
10. detection method according to claim 8 or claim 9, it is characterised in that in terms of g/mL, the cosmetic sample and second
The ratio of nitrile is 2:(10~20).
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| CN108828102A (en) * | 2018-08-20 | 2018-11-16 | 云南同创检测技术股份有限公司 | A kind of method of allyl cyclohexyl propionate and jasmine aldehyde in measurement flavors and fragrances |
| 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 |
| CN110174488A (en) * | 2019-06-10 | 2019-08-27 | 青岛农业大学 | A kind of Allergic skin test method 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 |
| CN115032312A (en) * | 2022-07-15 | 2022-09-09 | 浙江省产品质量安全科学研究院 | Method for simultaneously detecting multiple allergic aromatics in mosquito repellent product |
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