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日用化学工业（中英文）

日用化学工业（中英文） ›› 2025, Vol. 55 ›› Issue (2): 253-261.doi: 10.3969/j.issn.2097-2806.2025.02.015

• 分析与检测 • 上一篇    下一篇

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

李若绮1,孙莺1,*(),李莉1,魏学冰1,郭朝晖1,王任其2   

  1. 1.甘肃省药品检验研究院，甘肃 兰州 730070
    2.陕西科技大学，陕西 西安 710016
  • 收稿日期:2024-03-09 修回日期:2025-02-05 出版日期:2025-02-22 发布日期:2025-02-28
  • 通讯作者: 孙莺
  • 基金资助:
    甘肃省药品监督管理局药品科研项目(2022GSMPA0025);甘肃省科技厅重点研发项目(22YF7FA080);甘肃省委组织部重点人才项目;中国食品药品检定研究院技术开发项目

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

Ruoqi Li1,Ying Sun1,*(),Li Li1,Xuebing Wei1,Zhaohui Guo1,Renqi Wang2   

  1. 1. Gansu Institute for Drug Control, Lanzhou, Gansu 730070, China
    2. Shaanxi University of Science & Technology, Xi’an, Shaanxi 710016, China
  • Received:2024-03-09 Revised:2025-02-05 Online:2025-02-22 Published:2025-02-28
  • Contact: Ying Sun

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摘要：

建立了染发剂中6种染料的稳定同位素标记液质联用分析方法，选用丹磺酰氯和丹磺酰氯-D6为衍生化试剂，合理设计衍生化反应过程并优化衍生化反应条件，建立衍生化产物的多反应监测（MRM）方法，以丹磺酰氯-D6衍生化产物作为同位素内标对染料定性、定量分析。得到较佳衍生化反应条件：反应时间为50 min，反应温度为30 ℃和衍生化溶剂中三乙胺的添加量为20 μL。质谱分析采用电喷雾离子源正离子（ESI+）模式下多反应监测（MRM）方式。结果显示，6种染料衍生化产物的质量浓度范围为0.45~4.3 μg/mL，平均回收率为83.7%~114.3%，相对标准偏差（RSD）为2.3%~8.9%。结果表明该方法不仅提高了染料的稳定性，染料衍生化产物在4 ℃条件下，10天内化学性质稳定，还可排除强基质效应对染料准确定量分析，为禁限用染料的定性、定量分析提供新思路。

关键词: 染料, 稳定同位素标记, HPLC-MS/MS

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

中图分类号: 

  • TQ658