HPLC-MS/MS测定化妆品中5种禁用胆碱类化合物

doi:10.13218/j.cnki.csdc.2018.04.011

摘要/Abstract

摘要： 建立了高效液相色谱-质谱/质谱(HPLC-MS/MS)测定化妆品中5种禁用胆碱类化合物的分析方法。样品经甲醇-水(V(甲醇)∶V(水)=3∶1)溶液涡旋振荡、超声辅助液分散提取,离心后经Welch Ultimate XB-C₁₈ (4.6 mm×150 mm,5 μm)色谱柱分离。通过质谱电喷雾正离子模式(ESI⁺)电离、多反应监测模式(MRM)测定。在最优化条件下,5种禁用胆碱类化合物均获得良好分离,峰形对称性好。水杨酸胆碱在10.0~80.0 μg/L范围内线性良好,相关系数为0.999 1,其他胆碱在1.0~40.0 μg/L范围内线性良好,相关系数大于0.995 0;方法检出限和定量限分别在2.0~30.0 μg/kg 和6.0~90.0 μg/kg之间。添加回收实验结果表明,5种胆碱类化合物的回收率在85.4%~103.9%之间,日内精密度为1.9%~6.9% (n=6)。

关键词: 化妆品, 胆碱类化合物, 液相色谱-质谱/质谱法

Abstract: A method was developed for the determination of five kinds of choline compounds prohibited in cosmetics by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).The samples were oscillated and extracted with methanol-water solution (V(CH₃OH)∶V(H₂O)=3∶1) assisted by vortex and ultrasonic.Then,after centrifugation,the five target compounds were separated by Welch Ultimate XB-C₁₈ column (4.6 mm×150 mm,5 μm).The analytes were ionized by electrospray ionization in positive mode (ESI⁺) and detected under MRM mode.Under the optimal conditions,the five choline compounds prohibited are all well separated with good symmetry of peaks.The choline salicylate shows good linear relationship in the concentration range of 10.0-80.0 μg/L with correlation coefficient of 0.999 1.Other choline compounds show good linear relationship in the concentration range of 1.0-40.0 μg/L with the correlation coefficients larger than 0.995 0.The limits of detection and quantification (LOD and LOQ) of the method are in the range of 2.0-30.0 μg/kg and 6.0-90.0 μg/kg,respectively.The recovery experiments of spiked samples show that,the recoveries of the five choline compounds are in the range of 85.4%-103.9% with RSDs ranging from 1.9% to 6.9% (n=6).

Key words: cosmetics, choline compound, HPLC-MS/MS

中图分类号:

TQ658

张瑞瑞, 杜伟锋, 岑建斌, 区硕俊, 寻知庆, 黄金凤. HPLC-MS/MS测定化妆品中5种禁用胆碱类化合物[J]. 日用化学工业, 2018, 48(4): 237-242.

ZHANG Rui-rui, DU Wei-feng, CEN Jian-bin, OU Shuo-jun, XUN Zhi-qing, HUANG Jin-feng. Determination of five kinds of choline compounds prohibited in cosmetics by HPLC-MS/MS[J]. China Surfactant Detergent & Cosmetics, 2018, 48(4): 237-242.

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