CN101545891A - Method for concurrent measurement of p-phenylenediamine, o-phenylenediamine, hydroquinone and resorcinol in oxygenize type hair dyes agent - Google Patents
Method for concurrent measurement of p-phenylenediamine, o-phenylenediamine, hydroquinone and resorcinol in oxygenize type hair dyes agent Download PDFInfo
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- CN101545891A CN101545891A CN200910115246A CN200910115246A CN101545891A CN 101545891 A CN101545891 A CN 101545891A CN 200910115246 A CN200910115246 A CN 200910115246A CN 200910115246 A CN200910115246 A CN 200910115246A CN 101545891 A CN101545891 A CN 101545891A
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Abstract
The invention provides a method for concurrent measurement of p-phenylenediamine, o-phenylenediamine, hydroquinone and resorcinol in oxygenize type hair dyes agent, which includes hereafter steps: (1) confecting standard product solution of different coloring agent and differentmultiplying power content, (2) confecting the solution of need-checking sample, (3) respectively accurately extracting standard product solution and need-checking sample solution, injecting into the gas chromatography and taking measurement. In this invention, the fore treatment of the sample in this invention is easy, can save time and be easy to operate by employing capillary column, can synchronously detect the four oxygenize type coloring agent, can take quantitative analysis and reduce the cost, and has the feature of quick detecting.
Description
Technical field
The invention belongs to the chemical apparatuses analysis technical field, relate in a kind of oxidative hair dyes to, o-phenylenediamine with to, four kinds of dyestuffs of resorcinol methods for measuring simultaneously.
Background technology
Hair dye is a kind of cosmetics to hair-dyeing.According to the light industry standard QB/T of the People's Republic of China (PRC) 1978-2004 " hair dyes " regulation, hair dye can be divided into by dyeing theory: oxidative hair dyes and non-oxidative hair dye.
The oxidative coloration of hair agent is the main product on the market as a kind of Permanent Hair Dyeing Agent.Its principle be its used be the dyestuff intermediate of low relative molecular mass, as p-phenylenediamine (PPD), mutual-amino phenol etc.These dyestuff intermediates itself are colourless, can not use separately, oxidized generation quinone imines (P-benzoquinoneimine) when it mixes use with developer, generate diphenylamine (diphenylamine) with false carbanion coupling agent reaction again, this compound is further generated coloured macromolecular compound after the oxidation, thereby plays the effect of dyeing.Because the big molecule of dyestuff is to generate by dyestuff intermediate and the reaction of coupling agent micromolecule in hair fiber.Therefore, when washing, the big molecule of the dyestuff of formation is to be not easy to be rinsed by the aperture of hair fiber.
Hair dye hair dyeing contact skin, and in the process of hair dyeing, also will heat, make the organic substance of benzene class enter capillary by scalp, arrive marrow with blood circulation then, the prolonged and repeated candidate stem cell that acts on causes cancerating of candidate stem cell, causes leukemic generation.And multiple disease such as that why hair dye can cause is allergic, leukaemia.P-phenylenediamine (PPD) is a kind of colorant that must use in the hair dye, is internationally recognized a kind of carcinogen.
The versions in 2007 " cosmetics health standard " of health ministry issuing and implementation on July 1st, 2007.Standard has been listed and has been allowed 96 kinds of hair dye raw materials using in the hair dyeing cosmetics, and clear and definite their restriction request for utilization and label for labelling regulation.The security of hair dyeing product is very important, and the use of some dyestuffs might produce carcinogenesis to skin in the hair dye.As: o-phenylenediamine, m-phenylene diamine and their N position substitutive derivative and its esters belong to and forbid component in the cosmetics; P-phenylenediamine (PPD) and N position substitutive derivative thereof are and limit the use of material in the components of cosmetics, its maximum acceptable concentration (MPC) in cosmetics is 6% (in free radical), limit the use of in hair dyeing and use oxidation colorant, when generally using, must indicate this product on the Product labelling and contain " phenylenediamine ".Because the frequency of utilization height of shampoo, long-term accumulated is easy to the healthy and safe of consumer threatened.
Conventional sense method for the p-phenylenediamine (PPD) in the oxidative hair dyes, o-phenylenediamine, p-dihydroxy-benzene, resorcinol mainly contains high performance liquid chromatography at present.China's 2007 editions " cosmetics health standards " classifies o-phenylenediamine, p-phenylenediamine (PPD), m-phenylene diamine in the oxidative hair dyes as and limits the use of material, stipulates that its maximum acceptable concentration (MPC) in cosmetics is in 6%, and its detection method also is a high performance liquid chromatography.Detection limit is low though high performance liquid chromatography has, the sensitivity for analysis advantages of higher, is put into the conventional sense method, and used instrument costliness, analysis cost height in use are restricted, and can not detect multiple different dyes simultaneously.The present invention comes therefrom.
Summary of the invention
The object of the invention be to provide a kind of in the oxidative hair dyes to, o-phenylenediamine with to, four kinds of dyestuffs of resorcinol methods for measuring simultaneously, solved in the prior art defectives such as four kinds of dyestuffs can not detect simultaneously, testing cost is higher, analysis cost is high, use is limited.
In order to solve these problems in the prior art, technical scheme provided by the invention is as follows:
A kind of in the oxidative hair dyes to, o-phenylenediamine with to, four kinds of dyestuffs of resorcinol methods for measuring simultaneously, it is characterized in that said method comprising the steps of:
(1) standard solution of preparation different dyes different multiplying content;
(2) preparation testing sample solution;
(3) accurately draw standard solution and testing sample solution respectively, inject gas chromatograph is measured promptly.
Preferably, described standard solution compound method is as follows:
Accurately take by weighing p-phenylenediamine (PPD), o-phenylenediamine, p-dihydroxy-benzene, four kinds of standard dye product of resorcinol respectively in right amount, the adding anhydrous sodium sulfite is anti-oxidant, is mixed with the standard reserving solution of 10mg/mL with appropriate solvent; The standard reserving solution that preparation is obtained dilutes the standard solution that different multiplying obtains different dyes different multiplying content.
Preferably, described testing sample solution is prepared according to following steps:
It is an amount of accurately to take by weighing the hair dye sample, adds anhydrous sodium sulfite, is mixed with the solution of 0.1g/mL with appropriate solvent; Ultrasonic Extraction 20～60min, centrifugal filtration, filtrate is testing sample solution.
Preferably, described solvent is an ethyl acetate solution.
Preferably, described method also comprises the standard solution inject gas chromatograph and is horizontal ordinate with standard dye product content, is ordinate with the peak height or the peak area of the standard dye product of different multiplying, the drawing standard curve.
Preferably, the chromatographic condition during described step (3) gas Chromatographic Determination is:
Flow rate of carrier gas: nitrogen flow rate: 0.8～1.1mL/min; Hydrogen flow rate: 20～40mL/min; Air velocity: 300～400mL/min; Injector temperature: 240～280 ℃; Sample size: 0.05～0.5 μ L; Be regardless of the original mold formula that flows to;
Adopt capillary column; The chromatographic column adopting temperature programme, 150～170 ℃ keep 20～60sec, be warming up to 180～200 ℃ with 35～50 ℃/min and keep 7～10min, be warming up to 190～210 ℃ with 8～12 ℃/min then and keep 2～3min, be warming up to 270～300 ℃ with 35～45 ℃/min then and keep 1～3min; Detector temperature: 270～300 ℃.
Preferably, the chromatographic condition during described step (3) gas Chromatographic Determination is:
Flow rate of carrier gas: nitrogen flow rate: 1mL/min; Hydrogen flow rate: 30mL/min; Air velocity: 350mL/min; Injector temperature: 250 ℃; Sample size: 0.2 μ L; Be regardless of the original mold formula that flows to;
Adopt capillary column; The chromatographic column adopting temperature programme, 160 ℃ keep 30sec, are warming up to 190 ℃ with 40 ℃/min and keep 9min, are warming up to 200 ℃ with 10 ℃/min then and keep 2.5min, are warming up to 280 ℃ with 40 ℃/min then and keep 2min; Detector temperature: 280 ℃.
Preferably, described chromatographic column is selected DB-170130m*0.32mm*0.25 μ m capillary column for use.
Preferably, described method is measured the retention time and the compound at each peak in the chromatogram that obtains and is: No. 1 peak, retention time are 6.119min, are acetate ester; No. 2 peaks, retention time are 9.522min, are o-phenylenediamine; No. 3 peaks, retention time are 10.399min, are p-phenylenediamine (PPD); No. 4 peaks, retention time are 12.459min, are p-dihydroxy-benzene; No. 5 peaks, retention time are 13.105min, are resorcinol.
In the technical solution of the present invention in the hair dye above-mentioned four kinds of oxidized form dyestuffs after the ethyl acetate ultrasonic Extraction, filter, filtrate is analyzed with gas chromatograph (fid detector), and is qualitative with retention time, with standard items peak height or peak area quantification.Detection limit and the quantitative limit of o-phenylenediamine, p-phenylenediamine (PPD), p-dihydroxy-benzene, resorcinol have been increased greatly by technical scheme of the present invention.Wherein detecting of o-phenylenediamine is limited to 30ug/mL, quantitatively be limited to detecting of 100ug/mL, p-phenylenediamine (PPD) and be limited to 30ug/mL, quantitatively be limited to detecting of 100ug/mL, p-dihydroxy-benzene and be limited to 30ug/mL, quantitatively be limited to detecting of 100ug/mL, resorcinol and be limited to 30ug/mL, quantitatively be limited to 100ug/mL.
The present invention adopts the capillary column direct injected to analyze four kinds of oxidized form compounds simultaneously.Have the following advantages:
1. though high performance liquid chromatography, gas chromatography-mass spectrography have so that detection limit is low, the sensitivity for analysis advantages of higher in the prior art, also are put into the conventional sense method, the used instrument costliness of its method, analysis cost height in use are restricted.
2. sample pre-treatments of the present invention is simple, adopts capillary column can save time and easy operating.
3. four kinds of oxidized form compounds of hair dye can detect simultaneously in the technical scheme of the present invention, can quantitative test when adopting typical curve in the optimal technical scheme, save cost, and have the advantage of fast detecting.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described:
The chromatogram that Fig. 1 obtains for the embodiment of the invention.
Wherein: No. 1 peak is an ethyl acetate, and No. 2 peaks are that p-phenylenediamine (PPD), No. 3 peaks are that o-phenylenediamine, No. 4 peaks are that p-dihydroxy-benzene, No. 5 peaks are resorcinol.
Embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are used to the present invention is described and are not limited to limit the scope of the invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
The detection of four kinds of oxidized form dyestuffs in embodiment 1 hair dye:
Reagent and sample
Anhydrous sodium sulfite (analyzing pure), ethyl acetate (HPLC), o-phenylenediamine, p-phenylenediamine (PPD), p-dihydroxy-benzene, resorcinol standard items: purity 〉=99%;
Instrument and equipment
Gas chromatograph Agilent 6890N (FID), chromatographic column J﹠amp; W 123-0732 DB-170130m*0.32mm*0.25 μ m, ultrasonic cleaner, hydro-extractor, the organic miillpore filter of 0.45 μ m, 1.0 μ L microsyringes
Method:
Chromatographic condition
Start chromatograph, carry out necessary adjusting to reach the instrument best operating condition, chromatographic condition is selected according to concrete condition, and reference conditions are:
(1) carrier gas nitrogen flow velocity: 1.0mL/min; Hydrogen flow rate: 30mL/min; Air velocity: 350mL/min.
(2) injector temperature: 250 ℃
(3) sample introduction pattern: do not shunt
(4) sample size: 0.2 μ L
(5) chromatogram column temperature: adopt temperature programme to keep 0.5min for 160 ℃, 160 ℃ are warming up to 190 ℃ with 40 ℃/min and keep 9min, and 190 ℃ are warming up to 200 ℃ with 10 ℃/min and keep 2.5min, and 200 ℃ are warming up to 280 ℃ with 40 ℃/min and keep 2min
(6) detecting device: FID (hydrogen ion flame detector)
(7) detector temperature: 280 ℃
Standard reserving solution
Take by weighing four kinds of oxidized form standard dyes of 100mg product (p-phenylenediamine (PPD), o-phenylenediamine, p-dihydroxy-benzene, resorcinol, by the product purity conversion), add the 100mg anhydrous sodium sulfite respectively, fully dissolve with chromatographically pure ethyl acetate, and being settled to 10.0mL with brown volumetric flask, 4 ℃ of refrigerators are preserved.
The drafting of typical curve
Get difference above-mentioned standard reserving solution (6.1) 0.10mL, 0.25mL, 0.50mL, 1.00mL, 2.00mL, insert in the brown volumetric flask of 10mL, add chromatographically pure ethyl acetate and be settled to scale, abundant mixing, form content with standard reserving solution and be respectively 0.1,0.25,0.5,1.0, the standard dye product series of 2.0g/L.
Accurately draw 0.2 μ L standard solution with 1.0 μ L microsyringes, inject gas chromatograph is a horizontal ordinate with standard dye product content, is ordinate with the peak height or the peak area of sample separately, the drawing standard curve.
Sample pre-treatments
Get 1mL drinks sample with, take by weighing 1.0g hair dye sample (being accurate to 1mg), add the 100mg anhydrous sodium sulfite, pipette chromatographically pure ethyl acetate and be added into the 10mL scale, fully mixing is inserted ultrasonic Extraction 30min in the ultrasonic cleaner, the centrifugal 10min of 3000rpm, get supernatant with the organic filtering with microporous membrane of 0.45 μ m, filtrate is analyte sample fluid.
Get 10mL scale tool plug centrifuge tube, take by weighing 1.0g hair dye sample (being accurate to 1mg), add the 100mg anhydrous sodium sulfite, pipette chromatographically pure ethyl acetate and be added into the 10mL scale, fully mixing is inserted ultrasonic Extraction 30min in the ultrasonic cleaner, the centrifugal 10min of 3000rpm, get supernatant with the organic filtering with microporous membrane of 0.45 μ m, filtrate is analyte sample fluid.
Sample determination
Accurately draw 0.2 μ L testing sample solution with 1.0 μ L microsyringes, inject gas chromatograph, each sample replication twice obtains chromatogram such as Fig. 1, wherein, and No. 1 peak, retention time is 6.119min, is acetate ester; No. 2 peaks, retention time are 9.522min, are No. 3 peaks of o-phenylenediamine, and retention time is 10.399min, is p-phenylenediamine (PPD); No. 4 peaks, retention time are 12.459min, are p-dihydroxy-benzene; No. 5 peaks, retention time are 13.105min, are resorcinol.Measure peak height or peak area and establishing criteria curve calculation mean value.Computing formula is as follows:
Wherein, C: the percentage composition of dyestuff (g/g) in the sample;
W: the quality of sample (g);
N: by the mass concentration (mg/L) of dyestuff in the sample liquid of finding on the typical curve
V: sample constant volume, mL (being 10mL in this standard)
The precision of embodiment 2 detection methods and the recovery are investigated
The precision of method
Getting each 0.2 μ L of 200 and 1000 μ g/mL p-phenylenediamine (PPD), o-phenylenediamine, p-dihydroxy-benzene, resorcinol standard solution analyzes, repeat 7 times, and the RSD that calculates two kinds of concentration of relative standard deviation (RSD) .4 kind compound height is 1.7%～4.6%, the results are shown in Table
Table 1 Precision test result (n=7)
The recovery of method is investigated:
Get L'Oreal's paste and liquid hair dye, measure sample, add the standard solution of 1000 μ g/mL respectively, and it is carried out pre-service by pre-treatment step, analyze by chromatographiccondition, parallel sample introduction 3 times, the scope that records sample recovery rate is 87.5%～107.7%, result such as table 2.
Table 2 hair dye recovery test result (n=3)
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (9)
1, a kind of in the oxidative hair dyes to, o-phenylenediamine with to, four kinds of dyestuffs of resorcinol methods for measuring simultaneously, it is characterized in that said method comprising the steps of:
(1) standard solution of preparation different dyes different multiplying content;
(2) preparation testing sample solution;
(3) accurately draw standard solution and testing sample solution respectively, inject gas chromatograph is measured promptly.
2, method according to claim 1 is characterized in that described standard solution compound method is as follows:
Accurately take by weighing p-phenylenediamine (PPD), o-phenylenediamine, p-dihydroxy-benzene, four kinds of standard dye product of resorcinol respectively in right amount, the adding anhydrous sodium sulfite is anti-oxidant, is mixed with the standard reserving solution of 10mg/mL with appropriate solvent; The standard reserving solution that preparation is obtained dilutes the standard solution that different multiplying obtains different dyes different multiplying content.
3, method according to claim 1 is characterized in that described testing sample solution prepares according to following steps:
It is an amount of accurately to take by weighing the hair dye sample, adds anhydrous sodium sulfite, is mixed with the solution of 0.1g/mL with appropriate solvent; Ultrasonic Extraction 20～60min, centrifugal filtration, filtrate is testing sample solution.
4, method according to claim 3 is characterized in that described solvent is an ethyl acetate solution.
5, method according to claim 1, it is characterized in that described method also comprises the standard solution inject gas chromatograph and is horizontal ordinate with standard dye product content, peak height or peak area with the standard dye product of different multiplying are ordinate, the drawing standard curve.
6, method according to claim 1, the chromatographic condition when it is characterized in that described step (3) gas Chromatographic Determination is:
Flow rate of carrier gas: nitrogen flow rate: 0.8～1.1mL/min; Hydrogen flow rate: 20～40mL/min; Air velocity: 300～400mL/min; Injector temperature: 240～280 ℃; Sample size: 0.05～0.5 μ L; Be regardless of the original mold formula that flows to;
Adopt capillary column; The chromatographic column adopting temperature programme, 150～170 ℃ keep 20～60sec, be warming up to 180～200 ℃ with 35～50 ℃/min and keep 7～10min, be warming up to 190～210 ℃ with 8～12 ℃/min then and keep 2～3min, be warming up to 270～300 ℃ with 35～45 ℃/min then and keep 1～3min; Detector temperature: 270～300 ℃.
7, method according to claim 1, the chromatographic condition when it is characterized in that described step (3) gas Chromatographic Determination is:
Flow rate of carrier gas: nitrogen flow rate: 1mL/min; Hydrogen flow rate: 30mL/min; Air velocity: 350mL/min; Injector temperature: 250 ℃; Sample size: 0.2 μ L; Be regardless of the original mold formula that flows to;
Adopt capillary column; The chromatographic column adopting temperature programme, 160 ℃ keep 30sec, are warming up to 190 ℃ with 40 ℃/min and keep 9min, are warming up to 200 ℃ with 10 ℃/min then and keep 2.5min, are warming up to 280 ℃ with 40 ℃/min then and keep 2min; Detector temperature: 280 ℃.
8, method according to claim 1 is characterized in that described chromatographic column selects DB-170130m*0.32mm*0.25 μ m capillary column for use.
9, method according to claim 1, it is characterized in that described method measures the retention time and the compound at each peak in the chromatogram that obtains and be: No. 1 peak, retention time are 6.119min, are acetate ester; No. 2 peaks, retention time are 9.522min, are o-phenylenediamine; No. 3 peaks, retention time are 10.399min, are p-phenylenediamine (PPD); No. 4 peaks, retention time are 12.459min, are p-dihydroxy-benzene; No. 5 peaks, retention time are 13.105min, are resorcinol.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680592A (en) * | 2012-06-08 | 2012-09-19 | 上海市计量测试技术研究院 | Solution for measuring purity of para-phenylenediamine standard substance by using high performance liquid chromatograph and preparation method thereof |
| CN105467032A (en) * | 2015-12-10 | 2016-04-06 | 北京彤程创展科技有限公司 | Rapid quantitative analysis method for resorcinol in rubber adhesive R80 |
| CN107356695A (en) * | 2017-07-24 | 2017-11-17 | 北京泛博科技有限责任公司 | After oxidation dye dye in waste liquid dye content detection method and reuse method |
| CN111812265A (en) * | 2020-07-10 | 2020-10-23 | 甘肃省药品检验研究院 | Detection method for simultaneously determining 32 dyes in hair dye |
-
2009
- 2009-04-24 CN CN200910115246A patent/CN101545891A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680592A (en) * | 2012-06-08 | 2012-09-19 | 上海市计量测试技术研究院 | Solution for measuring purity of para-phenylenediamine standard substance by using high performance liquid chromatograph and preparation method thereof |
| CN105467032A (en) * | 2015-12-10 | 2016-04-06 | 北京彤程创展科技有限公司 | Rapid quantitative analysis method for resorcinol in rubber adhesive R80 |
| CN105467032B (en) * | 2015-12-10 | 2018-06-01 | 北京彤程创展科技有限公司 | The quick quantitative analytic method of resorcinol in gum cement R80 |
| CN107356695A (en) * | 2017-07-24 | 2017-11-17 | 北京泛博科技有限责任公司 | After oxidation dye dye in waste liquid dye content detection method and reuse method |
| CN111812265A (en) * | 2020-07-10 | 2020-10-23 | 甘肃省药品检验研究院 | Detection method for simultaneously determining 32 dyes in hair dye |
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