CN101625340A - High performance liquid chromatogram detecting method for detecting metaphenylene diamine in cosmetic oxidizing-type hair colorant - Google Patents
High performance liquid chromatogram detecting method for detecting metaphenylene diamine in cosmetic oxidizing-type hair colorant Download PDFInfo
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- CN101625340A CN101625340A CN200910040567A CN200910040567A CN101625340A CN 101625340 A CN101625340 A CN 101625340A CN 200910040567 A CN200910040567 A CN 200910040567A CN 200910040567 A CN200910040567 A CN 200910040567A CN 101625340 A CN101625340 A CN 101625340A
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Abstract
The invention aims at providing an analysis method for detecting metaphenylene diamine in a cosmetic oxidizing-type hair colorant. The method utilizes a high performance liquid chromatograph, thereby not only being capable of conducting correct qualitative analysis to metaphenylene diamine in the cosmetic oxidizing-type hair colorant but also being capable of microscale quantitative analysis. In the method, acetonitrile and triethanolamine are mixed to prepare a mixed solution for extracting the metaphenylene diamine in the cosmetic oxidizing-type hair colorant; after a series of operations such as ultrasonic extraction, centrifuging, filtration and the like, solid impurities are filtered out; the filtrate obtained from the filtration is defecated, and prepared sample liquid is placed on a machine; acetonitrile-triethanolamine buffering solution is used for elution and separation; and under a wavelength of 190-380 nm, data is collected and analyzed. The high performance liquid chromatograph is mainly provided with an inverse-phase C18 chromatographic column which takes stearyl silane bonding silica gel as filler, an ultraviolet detector or a diode array detector.
Description
Technical field:
The present invention is a new technology of utilizing high performance liquid chromatograph to detect m-phenylene diamine in the cosmetic oxidizing-type hair, is particularly useful for the qualitative and quantitative test of micro-m-phenylene diamine in the hair dye.
Background technology:
Hair dye can be divided into oxidized form (permanent) hair dye, direct type (temporary or semipermanent) hair dye, metallic salt hair dye, natural plant hair dye etc.During hair dyeing, pigment or pigment intermediate make 21 carbon fatty acid monothioester bond ruptures on hair cuticle F one deck by alkaline matter and superoxide, directly advance macrofibril and microfibril in people's hair cortex, therefrom carry out hair dye that oxidative polymerization forms new compound and be called oxidized form and send out agent.Wherein oxidative hair dyes accounts for 80% of market share so that its Color is good, tonal variation is wide, hold time plurality of advantages such as long and become most popular hair dye in the Europe and the U.S..Different with the hair dye of other type, oxidative hair dyes is formed by two doses, and mixing before using in hair chemical reaction takes place and produces color.Oxidative hair dyes is mainly by oxidized form dyestuff, oxygenant with auxilliaryly add agent etc. and form.The oxidized form dyestuff is made up of dyestuff former and coupling agent.Dyestuff former mainly comprises p-phenylenediamine (PPD) (PPD), p-aminophenol, toluene diamine (PTD) etc. and their isomeride and derivant.The preparation of aromatic amine derivatives of position between coupling agent mainly refers to is as resorcinol, m-phenylene diamine, meta-aminophenol etc. and homolog and derivant.Dyestuff former earlier and oxidant reaction generation coupling reaction and generate the dyestuff of various color and lusters such as macromolecular indoles under the effect of coupling agent again then.These water-fast dyestuffs cover hair surface on the one hand, infiltrate medula inside on the other hand, reach the effect of permanent hair dyeing.The dyestuff composition of different structure can make hair dye different colors.And wherein m-phenylene diamine belongs to the bigger article of toxicity, sucks its steam or dust and can cause asthma and other breathing problems.Skin absorbs and causes hematologic effects, influences kidney, liver function.It has nothing in common with each other to the reaction of skin, and acute eczema can be diffused into back, face and belly, and the crust of similar erysipelas is arranged.The topmost harm of m-phenylene diamine is methaemoglobinaemia and carcinogenesis.When being exposed to the atmosphere that contains arylamine or contacting arylamine, mainly be that skin contacts or breathing enters in the body.The result causes the oxygen enriching system of blood to damage and causes air hunger.M-phenylene diamine is 300mg/Kg to the oral median lethal dose of small white mouse, and influencing dosage is 18mg/Kg.Therefore in order to protect the healthy and safe of cosmetics consumer, set up sensitive, accurately, efficiently, the detection method of m-phenylene diamine is very urgent and necessary in the cosmetic oxidizing-type hair fast.
Summary of the invention:
The purpose of this invention is to provide a kind of analytical approach that detects the m-phenylene diamine in the cosmetic oxidizing-type hair, this technology utilizes high performance liquid chromatograph not only can carry out qualitative analysis accurately to the m-phenylene diamine in the cosmetic oxidizing-type hair, but also can carry out the quantitative test of trace.
The present invention is with the m-phenylene diamine in the mixed solution extraction cosmetic oxidizing-type hair of acetonitrile and triethanolamine configuration, through sequence of operations such as ultrasonic extraction, centrifugal, filtrations, the filtering solid impurity, clarify up to filtrate, get machine on the sample liquid for preparing, carry out wash-out with acetonitrile-triethanolamine buffer solution and separate, image data is analyzed under the 190-380nm wavelength.The main configuration of used high performance liquid chromatograph comprises that octadecylsilane chemically bonded silica is anti-phase C18 chromatographic column, UV-detector or the diode array detector of filling agent.
The main analytical procedure of this sample method following "
1 sample pretreatment
Take by weighing a certain amount of cosmetics (oxidative hair dyes) and place the 25mL color-comparison tube that adds 1% sodium sulfite solution, vortex to matrix is disperseed, be settled to scale with moving phase, ultrasonic again 10-20min, extract is transferred in the centrifuge tube, the centrifugal 5min of 5000rpm/min, through 0.45 μ m membrane filtration, filtrate is as treating sample measuring liquid.
2 chromatographic conditions
(1) chromatographic column: with the octadecylsilane chemically bonded silica is the anti-phase C18 chromatographic column of filling agent;
(2) detecting device: UV-detector or diode array detector;
(3) detect wavelength: select for use the 190-380nm wavelength as detecting wavelength;
(4) moving phase:
Organic phase: acetonitrile
Water: triethanolamine: water=0.5～2%: 99.5%～98% (regulating pH=6.0-9.0) with phosphoric acid
Organic phase: water=5～10%: 95～90% as moving phase, the about 20min of balance chromatographic column,
Make baseline steady, retention time is fit under this condition, peak shape symmetry, degree of separation good (R＞1.5).
(5) flow velocity: 0.5～1.5mL/min;
(6) column temperature: 15～35 ℃.
3 density calculating methods
Be mixed with certain density titer with the m-phenylene diamine standard substance, 5 μ L volume sample introductions by external standard method, are done linear regression with peak area-concentration, draw equation of linear regression, utilize the m-phenylene diamine content in the calculated by peak area sample of m-phenylene diamine in this equation and the sample.
4 sample detection
(1) carries out sample pretreatment according to the method in 1, get the sample 5 μ L sample introductions of handling well; And then get the m-phenylene diamine standard solution 5 μ L sample introductions of debita spissitudo.
(2) detect according to the testing conditions in 2, obtain the chromatogram of sample and the chromatogram of m-phenylene diamine standard items respectively; The chromatogram of sample and the chromatogram of standard items are compared, it is close with the standard items retention time among the sample chromatogram figure that (error range: the chromatographic peak of standard items retention time ± 0.5min) is corresponding m-phenylene diamine composition, accuracy in order to ensure testing result, can carry out spectral analysis (spectral analysis is only applicable to diode array detector) to the preliminary chromatographic peak of determining, if, can further determine the m-phenylene diamine composition in the sample with the maximum absorption wavelength and the spectrogram feature similarity of standard items.
(3) chromatographic peak area of m-phenylene diamine in the sample is brought in the equation of linear regression in 3 into the concentration of m-phenylene diamine in the calculation sample.
Because cosmetics are of a great variety, matrix is complicated, can not get rid of the possibility that interference component and m-phenylene diamine go out the peak at one time fully.Adopt diode array detector can obtain the uv absorption spectra of m-phenylene diamine,,, can further confirm by maximum absorption wavelength and the spectrogram feature of analyzing the two with the spectrogram contrast of standard items.
Analytical approach of the present invention is accurate, easy, quick, and is highly sensitive, and selectivity, good reproducibility are applicable to the oxidative coloration of hair agent of various formulations.
Description of drawings
Fig. 1 sample chromatogram figure
Fig. 2 m-phenylene diamine standard items chromatogram
Fig. 3 sample spectra figure
Fig. 4 m-phenylene diamine standard items spectrogram
Fig. 5 m-phenylene diamine canonical plotting
Embodiment
The invention will be further elaborated below in conjunction with concrete embodiment, but do not limit the present invention:
1 material
1.1 instrument
Tianjin, island auto injection highly effective liquid phase chromatographic system: Ultimate AQ-C18 (50mm * 4.6mm, 5 μ m, post numbers 220801527) chromatographic column, the SPD-20A ultraviolet-visible detector, the SPD-M20A diode array, LC-20AB binary geopressure gradient pump, SIL-20A automatic sample handling system, CTO-20A column oven and LCsolution chromatographic work station.
1.2 reagent and sample
Acetonitrile (chromatographically pure) is a Merck company product; 95% ethanol (top grade is pure) is Tianjin section close europeanized reagent development centre product; Phosphoric acid (analyzing pure) is bought industrial and commercial industrial corporation product for Tian Jinjin; Triethanolamine (analyzing pure) is Tianjin good fortune chemical reagent in a morning factory product; Sodium sulphite (analyzing pure) is a Tianjin Da Mao chemical reagent factory product; Ultrapure water is produced by Milli-Q system.
The m-phenylene diamine standard items are purchased the SERVICE in CHEM, and lot number is 395-55B, and purity is 99.5%.
Test sample be wash black.
1.3 standard items storing solution
Precision takes by weighing 53.52mg m-phenylene diamine standard items (purity is 99.5%) and places the 50mL volumetric flask, add the 0.01g sodium sulphite, add a little 95% dissolve with ethanol, and be settled to scale with 95% ethanol, shake up, the standard solution that is mixed with concentration and is 1.065mg/mL is deposited standby in 4 ℃ of refrigerators as storing solution.
2 methods
2.1 chromatographic condition
Chromatographic column: Ultimate AQ-C18 (150mm * 4.6mm, 5 μ m)
Moving phase: adopt acetonitrile: (water: triethanolamine=98: 1)=5: 95 (water is transferred pH=7.7 with phosphoric acid), this moving phase baseline noise is little, and is 7.70 o'clock peak shape symmetries in the pH value, and degree of separation is good
Detect wavelength: 280nm.Through the 190-400nm length scanning, m-phenylene diamine has absorption maximum near 290nm, but in order to enlarge the scope of application of method, so select 280nm as detecting wavelength.
Flow velocity: 1.0mL/min
Column temperature: 25 ℃
2.2 sample pretreatment
The cosmetics (one wash black) that take by weighing 1.00g place the 25mL color-comparison tube that adds 1% sodium sulfite solution 1.0mL, vortex to matrix is disperseed, be settled to scale with moving phase, ultrasonic again 15min, extract is transferred in the centrifuge tube, the centrifugal 5min of 5000rpm/min, through 0.45 μ m membrane filtration, filtrate is as treating sample measuring liquid.
2.3 sample detection
Get 5 μ L test liquid sample introductions, utilize the chromatographic condition in 2.1 to detect, obtain the chromatogram (Fig. 1) and the spectrogram (Fig. 3) of sample; The m-phenylene diamine standard items storing solution dilution of getting again in 1.3 is 106.50mg/L concentration, and 5 μ L sample introductions under the same testing conditions, obtain the chromatogram (Fig. 2) and the spectrogram (Fig. 4) of m-phenylene diamine standard items.
2.4 typical curve
The m-phenylene diamine storing solution is diluted to the standard series of following gradient concentration with moving phase: 26.63mg/L, 53.25mg/L, 106.50mg/L0,266.25mg/L, 532.50mg/L, get the standard solution 5 μ L sample introductions of each concentration, obtain the peak area (seeing Table 1) of each concentration, make peak area-concentration standard curve (see figure 5), obtain its equation of linear regression (finishing evaluation work) by the high performance liquid chromatography workstation.
Regression equation: A (Area)=3688.02*C-1078.3 R
2=0.9998
Table 1 m-phenylene diamine typical curve each point concentration and peak area
3 interpretations of result
By the chromatogram (Fig. 2) of m-phenylene diamine standard items as can be seen, the retention time of utilizing chromatogram testing conditions in 2.1 to obtain the m-phenylene diamine standard items is 5.335min, the chromatogram (Fig. 1) of sample and the chromatogram (Fig. 2) of standard items are compared, as seen the 5.315min place has the retention time 5.335min of a chromatographic peak and m-phenylene diamine standard items chromatographic peak close among the sample chromatogram figure, error is within ± 0.5 minute scope, therefore can determine tentatively that the chromatographic peak at 5.315min place among the sample chromatogram figure is a m-phenylene diamine, this peak area is 377722.The spectrogram (Fig. 3) at peak, 5.315min place among the sample chromatogram figure and the spectrogram (Fig. 4) of m-phenylene diamine standard items are compared, the maximum absorption wavelength of spectrogram that can find the spectrogram of sample and standard items is close, can determine further that retention time in the sample is that the component of 5.315min is a m-phenylene diamine.
In the chromatographic peak area 377722 substitution equations of linear regression with m-phenylene diamine in the sample, the content that can obtain m-phenylene diamine in the sample preparation liquid is 105.15mg/L (finishing computational engineering by the high performance liquid chromatography workstation), can get as calculated one wash black in m-phenylene diamine be 5258mg/kg.
Characteristics such as this invention has high resolving power, high sensitivity, reappearance, selectivity is good and sample pretreating method is simple, qualitative, the quantitative test of m-phenylene diamine in the suitable cosmetic oxidizing-type hair.
The present invention is a foundation with a large amount of experiments and theoretical analysis, find a kind of analytical approach of utilizing the efficient liquid phase chromatographic analysis instrument to detect m-phenylene diamine in the cosmetic oxidizing-type hair, filled up the research blank of m-phenylene diamine liquid-phase chromatographic analysis aspect in the cosmetic oxidizing-type hair.
Claims (8)
1. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine in the cosmetic oxidizing-type hair, it is characterized in that adopting UV-detector or diode array detector, with the external standard standard measure, adopting octadecylsilane chemically bonded silica is the C18 post of filling agent, with the m-phenylene diamine in the mixed solution extraction cosmetic oxidizing-type hair of acetonitrile and triethanolamine configuration, through ultrasonic extraction, centrifugal, sequence of operations such as filtration, the filtering solid impurity, clarify up to filtrate, get machine on the sample liquid for preparing, carry out wash-out with acetonitrile-triethanolamine buffer solution and separate, image data is analyzed under the 190-380nm wavelength.
2. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine is characterized in that adopting UV-detector or diode array detector in the cosmetic oxidizing-type hair according to claim 1.
3. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine in the cosmetic oxidizing-type hair according to claim 1, it is characterized in that adopting octadecylsilane chemically bonded silica is the C18 post of filling agent.
4. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine is characterized in that moving phase: organic phase: acetonitrile in the cosmetic oxidizing-type hair according to claim 1; Water: triethanolamine: water=0.5～2%: 99.5%～98% (regulating pH=6.0-9.0) with phosphoric acid; Organic phase: water=5～10%: 95～90% as moving phase.
5. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine in the cosmetic oxidizing-type hair according to claim 1 is characterized in that adopting under the 190-380nm wavelength image data to analyze, and optimal wavelength is 280nm.
6. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine is characterized in that flow velocity: 0.5～1.5mL/min in the cosmetic oxidizing-type hair according to claim 1; Column temperature: 15～35 ℃.Wherein optimum flow rate is 1.0mL/min, and optimum column temperature is 25 ℃.
7. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine in the cosmetic oxidizing-type hair according to claim 1, it is characterized in that sample pretreatment adopts the cosmetics take by weighing 1.00g (wash black) to place the 25mL color-comparison tube that adds 1% sodium sulfite solution 1.0mL, vortex to matrix is disperseed, be settled to scale with moving phase, ultrasonic again 15min is transferred to extract in the centrifuge tube, the centrifugal 5min of 5000rpm/min, through 0.45 μ m membrane filtration, filtrate is as treating sample measuring liquid.
8. the high-efficiency liquid chromatography method for detecting of m-phenylene diamine in the cosmetic oxidizing-type hair according to claim 1 is characterized in that behind the sample analysis utilizing external standard method to carry out quantitative test according to its peak area according to its retention time and spectrogram qualitative analysis.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101975831A (en) * | 2010-11-25 | 2011-02-16 | 中国检验检疫科学研究院 | Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) |
| CN107153102A (en) * | 2017-05-10 | 2017-09-12 | 江南大学 | A kind of method to be limited in amphiphilic polymers and surfactant composite micelle separation determination hair dye with dyestuff |
| 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 |
-
2009
- 2009-06-25 CN CN200910040567A patent/CN101625340A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101975831A (en) * | 2010-11-25 | 2011-02-16 | 中国检验检疫科学研究院 | Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) |
| CN101975831B (en) * | 2010-11-25 | 2012-09-05 | 中国检验检疫科学研究院 | Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) |
| CN107153102A (en) * | 2017-05-10 | 2017-09-12 | 江南大学 | A kind of method to be limited in amphiphilic polymers and surfactant composite micelle separation determination hair dye with dyestuff |
| 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 |
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Application publication date: 20100113 |