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Detection method for simultaneously determining 32 dyes in hair dye

A technology for hair dyes and dyes, which is applied in measuring devices, material separation, and analysis of materials, etc. It can solve problems such as low response value, unsatisfactory separation effect of hair dye sample matrix, and difficult qualitative analysis.

Active Publication Date: 2020-10-23
甘肃省药品检验研究院
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Thin layer chromatography cannot be accurately quantified, gas chromatography and gas chromatography-mass spectrometry are not conducive to the analysis of thermally unstable substances, and the hair dye sample matrix is ​​complex, the separation effect is not ideal, and qualitative difficulty
Although high-performance liquid chromatography-mass spectrometry has strong separation ability and high sensitivity, can reduce matrix effects and can quickly and accurately analyze target compounds, such methods are not included in the "Safety and Technical Specifications for Cosmetics" (2015 Edition) to detect Dye components, and the presence of hydroquinone, resorcinol, 2-methylresorcinol, 4-amino-3-nitrophenol, 4-chloro Resorcinol, 1,5-naphthalene diol, 2,7-naphthalene diol, 1-naphthol and other components have low response values, and the detection results are inaccurate, and the simultaneous detection of 32 dyes in hair dyes cannot be realized

Method used

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  • Detection method for simultaneously determining 32 dyes in hair dye
  • Detection method for simultaneously determining 32 dyes in hair dye
  • Detection method for simultaneously determining 32 dyes in hair dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1 measures the method of 32 kinds of dyestuffs in hair dye simultaneously

[0032] 1. Configuration of standard solution

[0033] 24 standard hair dyes (2-amino-3-hydroxypyridine, p-phenylenediamine, p-aminophenol, m-phenylenediamine, 2,6-diaminopyridine, m- Aminophenol, toluene-2,5-diamine sulfate, 2,4-diaminophenoxyethanol hydrochloride, 4-amino-m-cresol, N,N-di(2-hydroxyethyl)-p-phenyl Diamine sulfate, o-phenylenediamine, o-aminophenol, 2-chloro-p-phenylenediamine sulfate, phenylmethylpyrazolone, p-methylaminophenol sulfate, 2-nitro-p-phenylenediamine, 4-Amino-2-hydroxytoluene, 4-nitro-o-phenylenediamine, toluene-3,4-diamine, 6-amino-m-cresol, 6-oxindole, N,N-diethyl-terephthalene Amine sulfate, N,N-diethyltoluene-2,5-diamine hydrochloride and N-phenyl-p-phenylenediamine) each 15mg in the same 25mL volumetric flask, with methanol-2g / L bisulfite Sodium aqueous solution (volume ratio is 1:1) constant volume prepares the positive ion mixed standard stock s...

Embodiment 2

[0051] Embodiment 2 methodological verification

[0052] 1. Linear range and detection limit

[0053] A sample without 32 dye components was used as a blank matrix, and the peak area was taken as the ordinate (Y), and the corresponding substance concentration was taken as the abscissa (X), to establish a matrix addition curve. The results showed that due to the good ionization and specificity of the above compounds, the linear relationship of each component was good, and the correlation coefficient r was greater than 0.995. Taking the signal-to-noise ratio (S / N)=3 of the quantitative ion chromatographic peak as the limit of detection (LOD), and S / N=10 as the limit of quantification (LOQ), the detection of 24 dye components in the positive ion detection mode was obtained. The limit of detection is 0.0052-0.43mg / kg, and the limit of quantification is 0.018-1.5mg / kg; the detection limit of 8 dye components in negative ion detection mode is 0.022-2.4mg / kg, and the limit of quanti...

Embodiment 3

[0063] Embodiment 3 dyestuff stability analysis

[0064] Because the aniline and phenol molecules in the 32 dyes are easily oxidized, the stability analysis was carried out. The mixed standard solution of the same concentration (the concentration of 24 dye components in the positive ion detection mode is 5 mg / L, and the concentration of the 8 dye components in the negative ion detection mode is 20 mg / L) is continuously injected for 48 hours, and the phenylmethyl Pyrazolone is the only one among the 32 dyes that does not contain aniline and phenolic compounds, and has stable chemical properties. Taking p-phenylenediamine, p-aminophenol, N,N-di(2-hydroxyethyl)-p-phenylenediamine sulfate, m-aminophenol and 4-amino-2-hydroxytoluene as examples, positive ion detection mode The peak area of ​​the lower dye components changes with time as shown in image 3 As shown, the peak area of ​​the dye component increases with time in the positive ion detection mode, and the peak area increa...

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Abstract

The invention belongs to the technical field of cosmetic detection and particularly relates to a method for simultaneously determining 32 dyes in a hair dye by a high performance liquid chromatography-tandem mass spectrometry technology. The invention establishes a simple, convenient, rapid and high-throughput determination method, 32 dyes in the hair dye can be quantitatively determined at the same time, and the method has the advantages of simplicity in operation, high sensitivity, good recovery rate, good reproducibility, short detection time, low solvent consumption, high detection flux and high detection efficiency, and has very important significance for analyzing the quality safety of the hair dye.

Description

technical field [0001] The invention belongs to the technical field of cosmetic detection, and in particular relates to a detection method for simultaneous determination of 32 dyes in hair dyes by high performance liquid chromatography tandem mass spectrometry. Background technique [0002] Hair dye is a very common cosmetic. It belongs to special-purpose cosmetics in my country. It is divided into oxidative hair dye and non-oxidative hair dye. 80% of the hair dyes sold on the market are oxidative hair dyes. At present, more and more people like to dye their hair, and the consumers of hair dyes are getting younger and younger, so the safety of hair dyes has also attracted much attention. The hazards of hair dyes mainly come from dyes. The main components of dyes are aniline and phenolic compounds. These compounds are sensitizing and carcinogenic. Long-term use will cause chronic damage to human health. In recent years, studies have reported that hair dyes Use increases a pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/72
CPCG01N30/06G01N30/72G01N30/88G01N2030/884G01N2030/8845
Inventor 李若绮孙莺刘婷媛武悦杜兴
Owner 甘肃省药品检验研究院