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日用化学工业（中英文）

日用化学工业 ›› 2022, Vol. 52 ›› Issue (7): 785-790.doi: 10.3969/j.issn.1001-1803.2022.07.015

• 分析与检测 • 上一篇    下一篇

液相色谱-四极杆-飞行时间质谱法快速筛查化妆品中8种亚硝胺

蒋亚奇1,高天阳1,于海英1,李启艳1,*(),李军1,*(),谢亚平2   

  1. 1.山东省食品药品检验研究院 国家药品监督管理局化妆品原料质量控制重点实验室,山东 济南 250101
    2.SCIEX中国技术支持中心,北京 100015
  • 收稿日期:2021-11-02 修回日期:2022-06-29 出版日期:2022-07-22 发布日期:2022-07-21
  • 通讯作者: 李启艳,李军

Rapid screening and determination of eight nitrosamines in cosmetics by liquid chromatography-quadrupole-time-of-flight mass spectrometry

Jiang Yaqi1,Gao Tianyang1,Yu Haiying1,Li Qiyan1,*(),Li Jun1,*(),Xie Yaping2   

  1. 1. NMPA Key Laboratory for Quality Control of Cosmetics Raw Material, Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, China
    2. SCIEX, Analytical Instrument Trading Co., Ltd, Beijing 100015, China
  • Received:2021-11-02 Revised:2022-06-29 Online:2022-07-22 Published:2022-07-21
  • Contact: Qiyan Li,Jun Li

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摘要：

建立了液相色谱-四极杆-飞行时间质谱（LC-QTOF-MS）快速筛查和定量测定化妆品中8种亚硝胺的方法。化妆品经饱和氯化钠分散均匀后,加二氯甲烷涡旋提取,在室温下用氮气吹干二氯甲烷并以甲醇复溶后进样分析;待测物以甲醇和水作为流动相进行梯度洗脱,在Agilent Poroshell 120 SB-C18色谱柱上分离,采用大气压化学离子源,正离子信息依赖扫描（IDA）模式采集,同时获得了目标化合物的一级和二级质谱信息,采用Library view软件构建了8种亚硝胺的高分辨质谱数据库,将采集的结果与数据库比对实现了化妆品中8种亚硝胺的快速筛查。实验优化了样品前处理方法,经方法学考察,建立了化妆品中8种亚硝胺的含量测定方法。结果表明,与其他方法相比,该前处理方法既能达到净化目的,回收率还较高;在优化的条件下,8种亚硝胺在5~100 ng/mL范围内线性关系均良好（r≥0.999）;在高（0.50 mg/kg）、中（0.10 mg/kg）、低（0.03 mg/kg） 3个加标水平下,平均回收率在85.1%~113.1%之间,相对标准偏差（RSD）为1.4%~6.6%;检出限在0.001 0~0.020 0 mg/kg之间,定量限在0.003 0~0.060 0 mg/kg之间。该法前处理方式简便,分析时间短,可实现缺乏标准品的情况下对目标化合物的快速筛查,方法灵敏度和准确度均较高,适用于化妆品中痕量亚硝胺的检测。

关键词: 液相色谱-四极杆-飞行时间质谱, 亚硝胺, 快速筛查, 化妆品

Abstract:

A rapid screening and determination method was developed for eight nitrosamines in cosmetics by liquid chromatography-quadrupole-time-of-flight mass spectrometry. Cosmetics were well dispersed by saturated sodium chloride solution and extracted by vortex mixer using dichloromethane. After dichloromethane was dried under nitrogen, the residuums were redissolved by methanol; the separation of 8 target compounds was performed on an Agilent Poroshell 120 SB-C18 column with gradient elution using methanol and water as mobile phases. Detection was achieved by atmospheric pressure chemical ionization in the positive mode, and rapid screening could be achieved using high-resolution mass spectrometry database which was created and acquired by Library view 1.3.1 software. Sample pretreatment methods were optimized, and the determination method for 8 nitrosamines in cosmetics was established through methodological study. The results showed that: this sample pretreatment method had purifying effect and had a better recovery compared with other pretreatment methods; the eight nitrosamines all showed good linear relationship （r≥0.999） in the range of 5-100 ng/mL under the optimized conditions; the average recoveries were in the range of 85.1%-113.1% at three spiked levels （0.03, 0.10, 0.50 mg/kg） with relative standard deviations （RSDs） of 1.4%-6.6%; limits of detection （LODs） were in the range of 0.001 0-0.020 0 mg/kg, and limits of quantitation （LOQs） were in the range of 0.003 0-0.060 0 mg/kg. This method was simple and timesaving for rapid screening of target compounds even in case of lack of standards, and the method also had high sensitivity and accuracy, which was suitable for trace detection of nitrosamines in cosmetics.

Key words: liquid chromatography-quadrupole-time-of-flight mass spectrometry, nitrosamine, rapid screening, cosmetics

中图分类号: 

  • TQ658