安全监测

固相萃取净化-超高效液相色谱-三重四极杆/线性离子阱串联质谱法测定化妆品中16个卡因类组分*

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  • 江苏省食品药品监督检验研究院, 南京 210008
第一作者 Tel:(025)86251206;E-mail:flyluli@126.com

收稿日期: 2020-12-16

  网络出版日期: 2024-06-25

基金资助

*江苏省市场监督管理局科技计划项目(KJ207560)

Determination of 16 caine-type ingredients in cosmetics by UPLC-QQQ/LIT tandem mass spectrometry coupled with solid phase extraction*

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  • Jiangsu Institute for Food and Drug Control,Nanjing 210008, China

Received date: 2020-12-16

  Online published: 2024-06-25

摘要

目的:建立了固相萃取柱净化,超高效液相色谱-三重四极杆/线性离子阱串联质谱联用(UPLC- MS/MS)测定化妆品中添加的16个卡因类组分的方法。方法:不同基质样品用溶剂提取后,经Oasis MCX 固相萃取柱净化,采用ACE Excel 3 C18(150 mm×2.1 mm, 3.0 μm)分离16个卡因类组分,以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱。在电喷雾离子源(ESI)正离子模式下电离,多反应监测(MRM)模式下定量和线性离子阱增强子离子扫描(EPI)模式下定性。结果:16个卡因类组分在相应的测定范围内线性关系良好,相关系数(r)在0.999 5~1.000,在2个加标水平下,加标回收率范围为86.0%~113.2%,RSD (n=3)为0.9%~10.8%,各化学成分的检测下限在2~5 μg·kg-1。收集的59批次化妆品中15批次检出丙胺卡因、利多卡因、丁卡因,含量在16.4~150.2 mg·g-1结论:该方法简便,选择性好,灵敏度高,可用于化妆品中卡因类化学成分的定量测定和定性筛查。

本文引用格式

芦丽, 方方, 冯有龙, 曹玲 . 固相萃取净化-超高效液相色谱-三重四极杆/线性离子阱串联质谱法测定化妆品中16个卡因类组分*[J]. 药物分析杂志, 2021 , 41(12) : 2178 -2190 . DOI: 10.16155/j.0254-1793.2021.12.17

Abstract

Objective: To develop a method based on SPE-UPLC-MS/MS [solid phase extraction-ultraper-formance liquid chromatography (UPLC)-triple quadrupole mass spectrometry (QQQ)/ linear accelerated ion trap (LIT) tandem mass spectrometry mass spectrometry] for determination of 16 caine-type ingredients in cosmetics. Methods: Samples were extracted with solvent and then purified with an Oasis MCX column. 16 compounds were separated on an ACE Excel 3 C18(150 mm×2.1 mm, 3.0 μm)column with 0.1% formic acid solution-methanol as mobile phases by gradient elution. Detection was carried out by positive electrospray ionization (ESI+) mass spectrometer in multiple reaction monitor (MRM) mode for quantification and enhanced product ion(EPI) scan for qualification. Results: All the 16 caine-type ingredients showed good linearity in their reasonable ranges (r=0.999 5-1.000). The average recoveries of all compounds at two spiked levels were in the range of 86.0%-113.2% with RSDs (n=3) within 0.9%-10.8%. The LODs were all in the range of 2-5 μg·kg-1. Lidocaine,prilocaine and tracaine were found in 15 batches of the 59 tested samples. The contents were in range of 16.4-150.2 mg·g-1. Conclusion: With the advantages of rapidness, simplicity, good selectivity and high sensitivity, the method can be used for determination of caine-type ingredients in cosmetics.

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