染发剂中6种强还原性染料的稳定同位素标记液质联用分析方法

doi:10.3969/j.issn.2097-2806.2025.02.015

Abstract

Abstract:

A method was developed for analysis of stable isotope labeling of 6 dyes by HPLC-MS/MS. Using dansulfonyl chloride and dansulfonyl chloro-D6 as derivatization reagents, the derivatization reaction process was reasonably designed and the derivatization reaction conditions were optimized. A multiple response monitoring （MRM） method was established for the qualitative and quantitative analysis of dyes by using the derivations of dansulfonyl chloro-D6 as internal standard. Optimal derivatization reaction conditions: reaction time of 50 min, reaction temperature of 30 ℃, and addition of 20 μL of triethylamine in the derivatization solvent. Mass spectrometry analysis adopts multiple response monitoring （MRM） under ESI⁺mode of electrospray ion source. The concentrations of the six dye derivatives range from 0.45 to 4.3 μg/mL, with average recoveries ranging from 83.7% to 114.3% and relative standard deviations （RSD） ranging from 2.3% to 8.9%. The method not only improves the stability of dyes, but also eliminates the strong matrix effect for accurate quantitative analysis of dyes. The chemical properties of dye-derived products are stable within 10 days under the condition of 4 ℃. The establishment of this method provides a new idea for the qualitative and quantitative analysis of prohibited dyes.

Key words: dyes, stable isotope labeling, HPLC-MS/MS

CLC Number:

TQ658

Ruoqi Li,Ying Sun,Li Li,Xuebing Wei,Zhaohui Guo,Renqi Wang. A method for analysis of stable isotope labeling of 6 kinds of strongly reducing dyes in hair dyes by HPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2025, 55(2): 253-261.

Figures/Tables 12

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References 23

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No.	Compound	Q1 mass/（m/z）	Q3 mass/（m/z）	Retention time/min	DP/V	CE/V
1	p-苯二胺衍生化产物	342.4	108.0^* 170.2	3.14	80 80	30 30
2	p-苯二胺衍生化产物^*	348.4	108.0^* 176.7	3.36	80 80	30 30
3	m-苯二胺衍生化产物	342.4	108.0^* 170.2	4.68	80 80	30 30
4	m-苯二胺衍生化产物^*	348.4	108.0^* 176.7	4.54	80 80	30 30
5	o-苯二胺衍生化产物	342.4	108.0^* 170.2	6.20	80 80	30 30
6	o-苯二胺衍生化产物^*	348.4	108.0^* 176.7	6.14	80 80	30 30
7	p-氨基苯酚衍生化产物	343.4	171.0^* 235.9	7.36	60 60	32 32
8	p-氨基苯酚衍生化产物^*	349.4	177.0^* 242.0	7.48	60 60	32 32
9	m-氨基苯酚衍生化产物	343.4	171.2^* 233.0	5.54	60 60	35 35
10	m-氨基苯酚衍生化产物^*	349.4	177.0^* 233.0	5.46	60 60	35 35
11	o-氨基苯酚衍生化产物	343.4	171.0^* 235.9	8.58	60 60	32 32
12	o-氨基苯酚衍生化产物^*	349.4	177.0^* 242.0	8.57	60 60	32 32

No.	Compound	Recovery/%			RSD/%
No.	Compound	C1	C2	C3	C1	C2	C3
1	p-苯二胺衍生化产物	111.0	100.7	112.8	2.6	2.5	3.1
2	m-苯二胺衍生化产物	95.5	96.8	107.6	2.3	2.8	3.7
3	o-苯二胺衍生化产物	98.5	87.1	105.4	4.8	4.1	4.9
4	p-氨基苯酚衍生化产物	114.3	99.8	95.5	3.3	5.9	8.9
5	m-氨基苯酚衍生化产物	93.8	83.7	107.8	3.8	3.9	2.5
6	o-氨基苯酚衍生化产物	106.9	90.0	101.3	2.7	6.6	6.9

	p-苯二胺衍生化产物	m-苯二胺衍生化产物	o-苯二胺衍生化产物	p-氨基苯酚衍生化产物	m-氨基苯酚衍生化产物	o-氨基苯酚衍生化产物
LOD/ （mg/kg）	0.026	0.025	0.056	0.056	0.056	0.011
LOQ/ （mg/kg）	0.09	0.09	0.18	0.18	0.18	0.04

样品编号	含量/%
样品编号	p-苯二胺	m-苯二胺	o-苯二胺	p-氨基苯酚	m-氨基苯酚	o-氨基苯酚
样品1				0.071
样品2					0.024
样品3				0.074
样品4				0.021
样品5	0.025
样品6					0.017
样品7					0.210
样品8	0.270
样品9	0.270
样品10				0.240
样品11	0.680				0.130
样品12	0.360			0.069	0.069
样品13	0.130

A method for analysis of stable isotope labeling of 6 kinds of strongly reducing dyes in hair dyes by HPLC-MS/MS

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