CN109541047A - A kind of remaining method of methacrylate monomers in measurement cosmetics - Google Patents
A kind of remaining method of methacrylate monomers in measurement cosmetics Download PDFInfo
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- CN109541047A CN109541047A CN201811187479.9A CN201811187479A CN109541047A CN 109541047 A CN109541047 A CN 109541047A CN 201811187479 A CN201811187479 A CN 201811187479A CN 109541047 A CN109541047 A CN 109541047A
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- methacrylate monomers
- methacrylate
- remaining method
- cosmetics
- measurement
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of remaining methods of methacrylate monomers in measurement cosmetics, comprising the following steps: the sample for a) weighing 0.5g is diluted to 10mL with acetone, obtains processing sample；B) processing sample 4000rpm is centrifuged 10min, obtains centrifuged supernatant；C) 1mL centrifuged supernatant is taken to analyze by analysis machine, the application is simple and quick, it is reproducible, selectivity is strong, quasi-, reliably, it is sensitive, under 100 and 1000mg/kg spiked levels, the rate of recovery of methacrylate fully meets the methacrylate retention analysis work in nail-care products between 105.9%~124.4%.
Description
[technical field]
The present invention relates to the technical field of cosmetics detection, methacrylate monomers in especially a kind of measurement cosmetics
The technical field of remaining method.
[background technique]
Methacrylate (methyl methacrylate) is commonly used for the polymerization reaction production synthesis tree by monomer
Rouge, German federal risk assessment agency (BfR) have confirmed that there are the monomer chemistries of high-content in some import nail-care products
Substance.Methacrylate can cause contact hypersensitivity, and the growth of nail is interfered by inflammation, using containing highly concentrated
The nail-care products for spending methacrylate in the process can cause damages to health.Although polymer be it is safe, monomer is residual
Stay substance that can still be present in nail-care products.Other acrylate, such as ethyl methacrylate or hydroxyethyl methacrylate, all
It can cause contact dermatitis and Ocular irritation.German federal risk assessment agency (BfR) issues nail-care products manufacturer and reminds,
It is required that avoiding using monomers methyl methacrylate in self-hardening two kinds of powder or liquid component.
Since the constituent of cosmetics is complicated, when directly being measured to the methacrylate residual in sample, pass
The GC detector such as FID of system cannot be met the requirements at sensitivity, anti-interference aspect.And headspace analysis also has limitation, in addition to examining
Consider the boiling point of target components, the influence of component chemical property itself is also most important.Methacrylate monomers are although volatile,
But easily it polymerize under the conditions ofs illumination, heating etc., therefore headspace sampling can not meet analysis and require.It is, therefore, desirable to provide one
The remaining method of methacrylate monomers in accurate, reliable, the sensitive measurement cosmetics of kind.
[summary of the invention]
The object of the invention is to solve the problems of the prior art, a kind of accurate, reliable, sensitive measurement makeup is proposed
The remaining method of methacrylate monomers in product.
To achieve the above object, the invention proposes the remaining sides of methacrylate monomers in a kind of measurement cosmetics
Method, comprising the following steps:
A) sample for weighing 0.5g is diluted to 10mL with acetone, obtains processing sample；
B) processing sample 4000rpm is centrifuged 10min, obtains centrifuged supernatant；
C) 1mL centrifuged supernatant is taken to analyze by analysis machine.
Preferably, the acetone is chromatography pure acetone.
Preferably, the analysis machine is gas chromatograph-mass spectrometer GCMS.
Preferably, the gas chromatograph-mass spectrometer GCMS analysis condition are as follows: chromatographic column: Rtx-5Sil ms, 30m × 0.25mm
×0.25μm；Injector temperature: 250 DEG C；Column temperature program: 35 DEG C of holding 5min of initial temperature, then 30 DEG C/min is raised to 280 DEG C of holdings
2min；Pressure: constant pressure 51.9kPa；Input mode: split sampling, split ratio: 30:1；Ion source: 200 DEG C；Transmission line: 250
℃；Detector voltage: 0.9kV；Solvent clipping time: 2.5min.
Preferably, further including that standard curve is established.
Beneficial effects of the present invention: the present invention is by diluting sample with acetone, then through the laggard promoting the circulation of qi matter of centrifugal treating
Combined instrument GCMS analysis, this method are simple and quick, accurate, reliable, sensitive.
Feature and advantage of the invention will be described in detail by embodiment combination attached drawing.
[Detailed description of the invention]
Fig. 1 to Fig. 3 is that the standard of methyl methacrylate, ethyl methacrylate and hydroxyethyl methacrylate is bent respectively
Line chart.
[specific embodiment]
The remaining method of methacrylate monomers in a kind of measurement cosmetics of the present invention, comprising the following steps:
A) sample for weighing 0.5g is diluted to 10mL with acetone, obtains processing sample；
B) processing sample 4000rpm is centrifuged 10min, obtains centrifuged supernatant；
C) 1mL centrifuged supernatant is taken to be analyzed by gas chromatograph-mass spectrometer GCMS, analysis condition are as follows: chromatographic column: Rtx-
5Sil ms, 30m × 0.25mm × 0.25 μm；Injector temperature: 250 DEG C；Column temperature program: 35 DEG C of holding 5min of initial temperature, then 30
DEG C/min is raised to 280 DEG C of holding 2min；Pressure: constant pressure 51.9kPa；Input mode: split sampling, split ratio: 30:1；Ion
Source: 200 DEG C；Transmission line: 250 DEG C；Detector voltage: 0.9kV；Solvent clipping time: 2.5min；Acquisition mode: SIM acquisition.
SIM acquisition condition is shown in Table 1
1 methacrylate component retention time of table and SIM parameter
Standard solution is prepared:
A certain amount of each methacrylate standard items are weighed, are diluted to that 1000 μ g/mL are mixed to be denoted as to use liquid with acetone
It is spare.
Standard curve:
The mixed methyl acrylate standard for the use of liquid acetone difference compound concentration being 1,5,10,20,50,100 μ g/mL
Solution.Using concentration as abscissa, for peak area as ordinate, it is as shown in Figure 1 to Figure 3 to draw standard curve, related coefficient and
Detection limit is shown in Table 2.
Each methacrylate related coefficient of table 2 and minimum detectability (LOD)
| Number | Compound name | Correlation coefficient r | LOD(μg/mL) |
| 1 | Methyl methacrylate | 0.9989 | 0.129 |
| 2 | Ethyl methacrylate | 0.9986 | 0.111 |
| 3 | Hydroxyethyl methacrylate | 0.9981 | 0.060 |
Reperformance test:
The methacrylate mixed standard solution of 5 μ g/mL is prepared using acetone, is repeated sample introduction 6 times, repeated result is shown in
Table 3.
3 peak area repeatability result of table
Rate of recovery test:
Methacrylate mixed standard solution is added in the varnish base of blank respectively, addition concentration is 100 Hes
1000mg/kg, 3 parts of parallel processing respectively, recovery of standard addition (3 Duplicate Samples average recovery rates and RSD%) the results are shown in Table 4.
4 recovery of standard addition of table
Qualitative and quantitative analysis, the party are carried out to 3 kinds of methacrylate monomers residuals in nail polish using gas chromatograph-mass spectrometer
Method is simple and quick, reproducible, and selectivity is strong, quasi-, reliably, sensitive, under 100 and 1000mg/kg spiked levels, methyl
The rate of recovery of acrylate fully meets the methacrylate residual point in nail-care products between 105.9%~124.4%
Analyse work.
Above-described embodiment is the description of the invention, is not limitation of the invention, after any pair of simple transformation of the present invention
Scheme all belong to the scope of protection of the present invention.
Claims (5)
1. a kind of remaining method of methacrylate monomers in measurement cosmetics, it is characterised in that: the following steps are included:
A) sample for weighing 0.5g is diluted to 10mL with acetone, obtains processing sample；
B) processing sample 4000rpm is centrifuged 10min, obtains centrifuged supernatant；
C) 1mL centrifuged supernatant is taken to analyze by analysis machine.
2. the remaining method of methacrylate monomers in a kind of measurement cosmetics as described in claim 1, it is characterised in that:
The acetone is chromatography pure acetone.
3. the remaining method of methacrylate monomers in a kind of measurement cosmetics as described in claim 1, it is characterised in that:
The analysis machine is gas chromatograph-mass spectrometer GCMS.
4. the remaining method of methacrylate monomers in a kind of measurement cosmetics as claimed in claim 3, it is characterised in that:
The gas chromatograph-mass spectrometer GCMS-QP2010Ultra analysis condition are as follows: chromatographic column: the μ of Rtx-5Silms, 30m × 0.25mm × 0.25
m；Injector temperature: 250 DEG C；Column temperature program: 35 DEG C of holding 5min of initial temperature, then 30 DEG C/min is raised to 280 DEG C of holding 2min；Pressure
Power: constant pressure 51.9kPa；Input mode: split sampling, split ratio: 30:1；Ion source: 200 DEG C；Transmission line: 250 DEG C；Detector
Voltage: 0.9kV；Solvent clipping time: 2.5min；Acquisition mode: SIM acquisition.
5. the remaining method of methacrylate monomers in a kind of measurement cosmetics as described in claim 1, it is characterised in that:
It further include that standard curve is established.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811187479.9A CN109541047A (en) | 2018-10-12 | 2018-10-12 | A kind of remaining method of methacrylate monomers in measurement cosmetics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811187479.9A CN109541047A (en) | 2018-10-12 | 2018-10-12 | A kind of remaining method of methacrylate monomers in measurement cosmetics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109541047A true CN109541047A (en) | 2019-03-29 |
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| CN201811187479.9A Pending CN109541047A (en) | 2018-10-12 | 2018-10-12 | A kind of remaining method of methacrylate monomers in measurement cosmetics |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175799A (en) * | 2010-12-28 | 2011-09-07 | 西安航天三沃化学有限公司 | Method for testing contents of residual monomers in acrylate pressure sensitive adhesive by virtue of gas chromatography |
| CN103105437A (en) * | 2011-11-10 | 2013-05-15 | 中国检验检疫科学研究院 | Method for simultaneous determination of residual quantity of 8 ester allergenic aromatics in toys |
| CN103487542A (en) * | 2013-09-11 | 2014-01-01 | 湖南中烟工业有限责任公司 | Method for concurrently detecting 23 ester compounds in cigarette water-base adhesive |
| KR101734214B1 (en) * | 2014-09-26 | 2017-05-11 | 주식회사 엘지화학 | Analytical Method and System for Composition of Monomer in Modified (poly(vinylidene fluoride) Resin |
-
2018
- 2018-10-12 CN CN201811187479.9A patent/CN109541047A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175799A (en) * | 2010-12-28 | 2011-09-07 | 西安航天三沃化学有限公司 | Method for testing contents of residual monomers in acrylate pressure sensitive adhesive by virtue of gas chromatography |
| CN103105437A (en) * | 2011-11-10 | 2013-05-15 | 中国检验检疫科学研究院 | Method for simultaneous determination of residual quantity of 8 ester allergenic aromatics in toys |
| CN103487542A (en) * | 2013-09-11 | 2014-01-01 | 湖南中烟工业有限责任公司 | Method for concurrently detecting 23 ester compounds in cigarette water-base adhesive |
| KR101734214B1 (en) * | 2014-09-26 | 2017-05-11 | 주식회사 엘지화학 | Analytical Method and System for Composition of Monomer in Modified (poly(vinylidene fluoride) Resin |
Non-Patent Citations (4)
| Title |
|---|
| ZHOU, WANLONG 等: "Simultaneous determination of cosmetics ingredients in nail products by fast gas chromatography with tandem mass spectrometry", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 吕庆 等: "气相色谱-离子阱质谱联用测定玩具中8种酯类致敏性芳香剂", 《分析试验室》 * |
| 胡晓宇 等: "北京市28种美甲用品挥发性成分检测分析", 《卫生研究》 * |
| 赖莺 等: "微波辅助萃取-气相色谱-质谱法测定丙烯酸树脂中9种残余单体", 《色谱》 * |
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Application publication date: 20190329 |