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超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查染发剂中32种染料成分
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鞠玲燕,李兆杰,宋卫得,徐成钢,崔嘉 1.威海海关2.日照海关 
基金项目:原质检总局科研计划项目(2017IK223,2017IK220)
中文摘要:建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查和分析染发剂中32种禁限用染料的分析方法。样品经甲醇-2 g/L抗坏血酸水溶液溶解提取,正己烷净化,用ZORBAX Eclipse Plus C18(3.0 mm×100 mm,1.8 μm)色谱柱分离,以甲醇-5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,采用正、负离子切换同时测定了32种染料成分,显著提高了检测通量。以全扫描模式下提取的保留时间和一级母离子精确质量数以及同位素丰度比,实现对染发剂中多种染料成分的快速筛查;以自动触发采集的二级碎片离子精确质量数进行确证。32种染料在相应的质量浓度范围内线性关系良好,相关系数(r2)均大于0.99;定量下限(LOQ)为0.2~40 μg/g,回收率为81.0%~110%,相对标准偏差(RSD)为3.3%~9.9%。该方法简单、准确、快速,适用于染发剂中多种禁限用染料成分的高通量快速定性筛查和定量分析。
中文关键词:超高效液相色谱  静电场轨道阱高分辨质谱  染发剂  染料  快速筛查
 
Rapid Screening of 32 Dyes in Oxidative Hair Dyes by Ultra-performance Liquid Chromatography-Quadrupole/Electrostatic Field Obitrap High-resolution Mass Spectrometry
Abstract:A method was developed for the rapid screening and analysis of 32 banned and restricted components in hair dyes by ultra performance liquid chromatography-quadrupole/electrostatic field obitrap high resolution mass spectrometry.The samples were extracted using a mixed solution of methanol and 2 g/L aqueous ascorbic acid,and purified with n hexane.The separation was carried out on an ZORBAX Eclipse Plus C18 column(3.0 mm×100 mm,1.8 μm)by gradient elution with methanol and 5 mmol/L ammonium acetate as mobile phases.The 32 components were simultaneously analyzed in switching positive and negative modes.The retention time,accurate mass of parent ion and relative isotope abundance in full scan mode were used for fast screening of multi components in hair dyes,while accurate mass of fragment ions in two stage threshold triggered full mass scan mode were used for confirmation.Under the optimal conditions,good linearities(r2>0.99)were obtained in their respective concentration ranges.The limits of quantitation(LOQ)for 32 compounds were in the range of 0.2-40 μg/g.The recoveries ranged from 81.0% to 110% with relative standard deviations(RSDs)of 3.3%-9.9%.The method was simple,sensitive and accurate,and was suitable for the rapid screening and confirmation of 32 kinds of banned and restricted component in hair dyes.
Key Words:ultra-performance liquid chromatography  obitrap high resolution mass spectrometry  hair dyes  dye  rapid screening
引用本文:鞠玲燕,李兆杰,宋卫得,徐成钢,崔嘉.超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查染发剂中32种染料成分[J].分析测试学报,2019,(8):931-938.
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