CN103940922B - In a kind of cosmetics, five kinds of forbiddings remove the assay method of mite agent - Google Patents
In a kind of cosmetics, five kinds of forbiddings remove the assay method of mite agent Download PDFInfo
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- CN103940922B CN103940922B CN201410138423.XA CN201410138423A CN103940922B CN 103940922 B CN103940922 B CN 103940922B CN 201410138423 A CN201410138423 A CN 201410138423A CN 103940922 B CN103940922 B CN 103940922B
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 34
- 239000002537 cosmetic Substances 0.000 title claims abstract description 32
- 238000003556 assay Methods 0.000 title claims abstract description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 150000002825 nitriles Chemical class 0.000 claims abstract description 10
- 239000008188 pellet Substances 0.000 claims abstract description 10
- FBQQHUGEACOBDN-UHFFFAOYSA-N quinomethionate Chemical compound N1=C2SC(=O)SC2=NC2=CC(C)=CC=C21 FBQQHUGEACOBDN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims abstract description 4
- 238000002347 injection Methods 0.000 claims abstract description 4
- 239000007924 injection Substances 0.000 claims abstract description 4
- 238000010792 warming Methods 0.000 claims abstract description 4
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 3
- -1 polysiloxanes Polymers 0.000 claims abstract description 3
- 239000010453 quartz Substances 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 11
- 241000894006 Bacteria Species 0.000 abstract description 9
- 150000003851 azoles Chemical class 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000012224 working solution Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 206010012442 Dermatitis contact Diseases 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 230000003255 anti-acne Effects 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 208000010247 contact dermatitis Diseases 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005264 electron capture Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
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- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses five kinds of forbiddings in a kind of cosmetics and remove the assay method of mite agent, comprise the steps: that (1) adopts the ultrasonic extraction sample of methyl alcohol, extract is centrifugal, get supernatant and be dried, filter; (2) filtrate is carried out to gas Chromatographic Determination, chromatographic column adopting HP-5? the nonpolar quartz capillary column of 5% phenyl methyl polysiloxanes, 30m × 0.25mm (i.d.) × 0.25 μ m; Injector temperature: 220 DEG C; Flow velocity: 2mL/min; Temperature programming condition: 80 DEG C of initial temperatures, keep 1.5min, be warming up to 250 DEG C with 30 DEG C/min speed, keep 2min; Injection port split ratio is 5:1; Wherein, described five kinds of forbiddings except mite agent be Bravo, gram mould pellet, chinomethionat, nitrile bacterium azoles and difoltan. The method of the invention is accurate, reliable, easy, specificity and highly sensitive.
Description
Technical field
The present invention relates to a kind of detection method, particularly relate to a kind of mensuration of removing mite agent for five kinds of forbiddings of cosmeticsMethod.
Background technology
Along with the fast development of Chinese national economy and improving constantly of living standards of the people, cosmetics become daily day by dayThe indispensable necessity of living. China has become Cosmetic Manufacture and consumption big country at present, and cosmetic industry has also become meOne of industry with fastest developing speed in state's national economy. All with day in the face of the high speed development of cosmetic industry and cosmetics demandIncrease, the product quality of cosmetics and security are more and more subject to consumers in general's concern and attention. In cosmetics, may existChemical hazard material can have a strong impact on consumer's healthy and safe generation.
" European Union's cosmetics regulation " (EC1223/2009), China's " cosmetics health specification " (version in 2007) all clearly ruleFixed, five kinds of Bravo, gram mould pellet, chinomethionat, nitrile bacterium azoles and difoltan etc. except mite agent be banned substance in components of cosmetics. ChangingIn adornment product, illegal interpolation forbidding is except mite agent, although may play in a short time the effect except mite, anti-acne, long-term use can stimulate skinSkin, causes contact dermatitis, when serious, can cause drug resistance and healthy hidden danger, and therefore exploitation is set up forbidding in cosmetics and removed mite agentDetection method, very necessary for guaranteeing cosmetics quality safety.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of accurate, reliable, easy, specificity and highly sensitive cosmeticIn product, five kinds of forbiddings remove the assay method of mite agent.
In cosmetics, five kinds of forbiddings remove an assay method for mite agent, comprise the steps:
(1) pre-treatment of sample: adopt methyl alcohol as the ultrasonic extraction sample of extract, extract is centrifugal, draw supernatantLiquid drying, crosses 0.45 μ m miillpore filter, and filtrate is for subsequent use;
(2) filtrate obtaining is carried out to gas Chromatographic Determination, described gc analysis condition is as follows: chromatographic column: HP-The nonpolar quartz capillary column of 55% phenyl methyl polysiloxanes, 30m × 0.25mm (i.d.) × 0.25 μ m; Injector temperature:220 DEG C; Flow velocity: 2mL/min; Temperature programming condition: 80 DEG C of initial temperatures, keep 1.5min, be warming up to 30 DEG C/min speed250 DEG C, keep 2min; Injection port split ratio is 5:1; Dottle pin purge flow rate: 3mL/min; Sample size: 1 μ L; Detector: electronicsAcquisition detector; Make-up gas flow: 3mL/min; Wherein, described five kinds of forbiddings except mite agent be Bravo, gram mould pellet, chinomethionat,Nitrile bacterium azoles and difoltan.
In cosmetics of the present invention, five kinds of forbiddings remove the assay method of mite agent, and wherein, step (1) is specially: take1g cosmetic sample (being accurate to 0.01g), is placed in 10mL colorimetric cylinder, add methyl alcohol as extract to scale, put ultrasonic waveIn extractor after ultrasonic extraction 15min, described extract is poured in centrifuge tube with the centrifugal 10min of 12000r/min rotating speed, usedSuction pipe is drawn supernatant through anhydrous sodium sulfate drying, finally crosses 0.45 μ m miillpore filter, and filtrate is for gas Chromatographic Determination.
In cosmetics of the present invention, five kinds of forbiddings are except the assay method difference from prior art of mite agent: domestic at presentThere is not yet the assay method except mite agent of above-mentioned five kinds of forbiddings in cosmetics outward, in cosmetics of the present invention, five kinds of forbiddings are except the survey of mite agentThe method of determining is accurate, reliable, easy, specificity and highly sensitive, and the method that the present invention sets up can be the inspection of China's cosmeticsThe quality control of work and daily production provides effective scientific basis and technical support.
In cosmetics of the present invention, forbidding is except the assay method of mite agent, wherein, and when sampling 1g, Bravo, gram mould pellet,The method detection limit of chinomethionat, nitrile bacterium azoles and difoltan is respectively 0.1mg/kg, 5mg/kg, 0.1mg/kg, 1mg/kg, 10mg/Kg. Add under concentration levels at basic, normal, high three, five kinds of forbiddings are except the average recovery rate scope of mite agent is 91.6%～97.0%Between, relative standard deviation (RSD) is between 2.5%～6.2%
Below in conjunction with accompanying drawing, five kinds of forbiddings in cosmetics of the present invention are described further except the assay method of mite agent.
Brief description of the drawings
Fig. 1 is that in the inventive method, five kinds of forbiddings remove the chemical structural formula of mite agent;
Fig. 2 is that in the inventive method cosmetics, five kinds of forbiddings remove the gas chromatogram of mite agent.
Detailed description of the invention
Embodiment 1
In cosmetics, five kinds of forbiddings remove an assay method for mite agent, comprise the steps:
Five kinds of forbiddings such as Bravo, gram mould pellet, chinomethionat, nitrile bacterium azoles, difoltan remove the essential information of mite agent material in Table1, five kind of forbidding is shown in Fig. 1 except the chemical structural formula of mite agent.
Five kinds of forbiddings of table 1. are except the essential information of mite agent material
The preparation of series hybrid standard working solution: by methyl alcohol by Bravo, gram mould pellet, chinomethionat, nitrile bacterium azoles, difoltanBe mixed with respectively the standard reserving solution that concentration is 1000 μ g/mL, then become the mixing of concentration as shown in table 2 with methyl alcohol stepwise dilutionSeries standard working solution:
Five kinds of forbiddings of table 2. are except the compound concentration of the series standard working solution of mite agent
The pre-treatment of sample: take 1g cosmetic sample (being accurate to 0.01g), be placed in 10mL colorimetric cylinder, add methyl alcoholTo scale, put in ultrasonic extractor after ultrasonic extraction 15min, said extracted liquid is poured in centrifuge tube and turned with 12000r/minThe centrifugal 10min of speed, draws supernatant through anhydrous sodium sulfate drying with suction pipe, finally crosses 0.45 μ m miillpore filter, and filtrate is for gas phaseChromatographic determination;
Described gc analysis condition is as follows: chromatographic column: the nonpolar quartz wool of HP-55% phenyl methyl polysiloxanesCapillary column, 30m × 0.25mm (i.d.) × 0.25 μ m; Injector temperature: 220 DEG C; Flow velocity: 2mL/min; Temperature programming condition:80 DEG C of initial temperatures, keep 1.5min, are warming up to 250 DEG C with 30 DEG C/min speed, keep 2min; Injection port split ratio is 5:1;Dottle pin purge flow rate 3mL/min; Sample size: 1 μ L; Detector: electron capture detector; Make-up gas flow: 3mL/min; Wherein,Described five kinds of forbiddings, except mite agent is Bravo, gram mould pellet, chinomethionat, nitrile bacterium azoles and difoltan, can complete five kinds of forbiddings simultaneouslyExcept the mensuration of mite agent. As shown in Figure 2, wherein, the corresponding relation of each peak and each material is measurement result: 7.589min(hundred bacteriumClearly), 9.227min(gram mould pellet), 9.507min(chinomethionat), 10.669min(nitrile bacterium azoles), 12.522min(difoltan), thisIn invention five kinds of forbiddings except linear equation, coefficient correlation, instrument detection limit and the method detection limit of mite agent as shown in table 3.
Five kinds of forbiddings of table 3. are except linear equation, coefficient correlation, instrument detection limit and the method detection limit of mite agent
| Forbidding is except mite agent | Linear equation | Coefficient correlation | Instrument detection limit (μ g/mL) | Method detection limit (mg/kg) |
| Bravo | Y=22127X-29305 | 0.9967 | 0.01 | 0.1 |
| Gram mould pellet | Y=56440X-4311 | 0.9998 | 0.5 | 5 |
| Chinomethionat | Y=36502X-43623 | 0.9995 | 0.01 | 0.1 |
| Nitrile bacterium azoles | Y=13289X-1505 | 0.9997 | 0.1 | 1 |
| Difoltan | Y=22623X-470185 | 0.9949 | 1.0 | 10 |
Take after measured containing five kinds of forbiddings and be accurate to 0.01g except the blank cosmetic sample 1.0g(of mite agent), add respectivelyAdd the mixed standard solution of basic, normal, high three concentration, vortex vibration mixes, and the method for establishing in strict accordance with this experiment is dividedAnalyse mensuration, 6 parts of parallel determinations under each interpolation concentration level of every type of sample, carry out quantitatively with accompanying calibration curve,And calculate relative standard deviation (RSD), experimental result is in table 4. As seen from table, five kinds of forbiddings remove the average recovery rate of mite agentScope is between 91.6%～97.0%, and relative standard deviation (RSD) is between 2.5%～6.2%, and rate of recovery experimental result is satisfied,Can meet in cosmetics the mensuration requirement of five kinds of forbiddings except mite agent.
In table 4. cosmetics, five kinds of forbiddings remove the rate of recovery and the precision (n=6) of mite agent
Above-described embodiment is described the preferred embodiment of the present invention, not to model of the present inventionEnclose and limit, design under the prerequisite of spirit not departing from the present invention, those of ordinary skill in the art are to technical side of the present inventionVarious distortion and improvement that case is made, all should fall in the definite protection domain of the claims in the present invention book.
Claims (2)
1. in cosmetics, five kinds of forbiddings remove an assay method for mite agent, it is characterized in that: comprise the steps:
(1) pre-treatment of sample: adopt methyl alcohol as the ultrasonic extraction sample of extract, extract is centrifugal, draw supernatant warpDry, cross 0.45 μ m miillpore filter, filtrate is for subsequent use;
(2) filtrate obtaining is carried out to gas Chromatographic Determination, described gc analysis condition is as follows: chromatographic column: HP-55%The nonpolar quartz capillary column of phenyl methyl polysiloxanes, 30m × 0.25mm (i.d.) × 0.25 μ m; Injector temperature: 220DEG C; Flow velocity: 2mL/min; Temperature programming condition: 80 DEG C of initial temperatures, keep 1.5min, be warming up to 250 with 30 DEG C/min speedDEG C, keep 2min; Injection port split ratio is 5:1; Dottle pin purge flow rate: 3mL/min; Sample size: 1 μ L; Detector is that electronics is caughtObtain detector; Make-up gas flow 3mL/min; Wherein, described five kinds of forbiddings except mite agent be Bravo, gram mould pellet, chinomethionat, nitrile bacteriumAzoles and difoltan.
2. in cosmetics according to claim 1, five kinds of forbiddings remove the assay method of mite agent, it is characterized in that: step (1)Be specially: take 1g cosmetic sample, be accurate to 0.01g, be placed in 10mL colorimetric cylinder, add methyl alcohol extremely to carve as extractDegree, puts in ultrasonic extractor after ultrasonic extraction 15min, by described extract pour in centrifuge tube with 12000r/min rotating speed fromHeart 10min, draws supernatant through anhydrous sodium sulfate drying with suction pipe, finally crosses 0.45 μ m miillpore filter, and filtrate is for gas-chromatographyMeasure.
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| CN201410138423.XA CN103940922B (en) | 2014-04-08 | 2014-04-08 | In a kind of cosmetics, five kinds of forbiddings remove the assay method of mite agent |
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| CN109709231A (en) * | 2019-01-28 | 2019-05-03 | 中南大学 | The remaining determination method of Bravo in water environment |
| CN115267011B (en) * | 2022-09-06 | 2024-05-07 | 重庆市食品药品检验检测研究院 | Liquid chromatography-mass spectrometry chromatography method for qualitative detection of illegally added drugs in oil-control cosmetics |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103163265A (en) * | 2013-03-18 | 2013-06-19 | 中国农业科学院烟草研究所 | Method for determining residual quantity of myclobutanil by SPE-GC/ECD (Solid Phase Extraction-Gas Chromatography-Electron Capture Detector) |
| CN103353488A (en) * | 2013-06-19 | 2013-10-16 | 中华人民共和国潍坊出入境检验检疫局 | Method for determining residues of chlorothalonil, captan, captafol and folpet in vegetables and fruits |
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| AU2005278765A1 (en) * | 2004-08-30 | 2006-03-09 | Saika Technological Institute Foundation | Analytical method for organic chemical material utilizing solid phase cartridge, and apparatus therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103163265A (en) * | 2013-03-18 | 2013-06-19 | 中国农业科学院烟草研究所 | Method for determining residual quantity of myclobutanil by SPE-GC/ECD (Solid Phase Extraction-Gas Chromatography-Electron Capture Detector) |
| CN103353488A (en) * | 2013-06-19 | 2013-10-16 | 中华人民共和国潍坊出入境检验检疫局 | Method for determining residues of chlorothalonil, captan, captafol and folpet in vegetables and fruits |
Non-Patent Citations (2)
| Title |
|---|
| VANWELIE, RTH;VANDUYN, P;LAMME, EK.DETERMINATION OF TETRAHYDROPHTALIMIDE AND 2-THIOTHIAZOLIDINE-4-CARBOXYLIC ACID, URINARY METABOLITES OF THE FUNGICIDE CAPTAN, IN RATS AND HUMANS.《INTERNATIONAL ARCHIVES OF OCCUPATIONAL AND ENVIRONMENTAL HEALTH》.1991,第63卷(第3期),181-186. * |
| 气相色谱-质谱法测定化妆品中16种有机氯农药;周相娟，赵玉琪，许华;《分析试验室》;20131231;第32卷(第12期);74-78 * |
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