色谱

色谱 ›› 2017, Vol. 35 ›› Issue (11): 1145-1151.DOI: 10.3724/SP.J.1123.2017.08011

• 研究论文 • 上一篇    下一篇

中空纤维液相微萃取-超高效液相色谱-串联质谱法测定儿童玩具中6种致敏香豆素类化合物

胡明珠1, 连显会1,2, 刘晗1, 郭项雨1, 吕悦广1,3, 白桦1, 薛宏宇2, 马强1   

  1. 1. 中国检验检疫科学研究院, 北京 100176;
    2. 大连理工大学生命与医药学院, 辽宁 盘锦 124221;
    3. 中国科学院大学化学与化工学院, 北京 101407
  • 收稿日期:2017-08-16 出版日期:2017-11-08 发布日期:2014-01-17
  • 通讯作者: 马强,Tel:(010)53897463,E-mail:maqiang@caiq.gov.cn
  • 基金资助:

    国家重点研发计划（2016YFF0203701）.

Determination of six allergenic coumarin compounds in children's toys using hollow-fiber liquid-phase microextraction followed by ultra-performance liquid chromatography-tandem mass spectrometry

HU Mingzhu1, LIAN Xianhui1,2, LIU Han1, GUO Xiangyu1, LÜ Yueguang1,3, BAI Hua1, XUE Hongyu2, MA Qiang1   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
    2. School of Life Science and Medicine, Dalian University of Technology, Panjin 124221, China;
    3. School of Chemistry and Chemical Engineering, University of Chinese Academy of Sciences, Beijing 101407, China
  • Received:2017-08-16 Online:2017-11-08 Published:2014-01-17
  • Supported by:

    National Key Research & Development Program of China (No. 2016YFF0203701).

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139

被引次数

4

摘要：

建立了超高效液相色谱-串联质谱测定儿童玩具中6种致敏香豆素类化合物（香豆素、7-甲基香豆素、7-甲氧基香豆素、7-乙氧基-4-甲基香豆素、4，6-二甲基-8-叔丁基香豆素和六氢香豆素）的分析方法。样品前处理采用中空纤维液相微萃取技术，优化后的萃取实验条件为：萃取剂正辛醇，搅拌速度700 r/min，萃取时间50 min，氯化钠加入量0.7 g。萃取液经ACQUITY UPLC BEH Phenyl色谱柱（150 mm×2.1 mm，1.7 μm）分离，目标化合物在电喷雾离子源正离子模式下电离，采用多反应监测模式进行定性定量分析。结果表明，6种致敏香豆素类化合物的定量限为2 μg/kg（7-乙氧基-4-甲基香豆素、4，6-二甲基-8-叔丁基香豆素）或10 μg/kg（香豆素、六氢香豆素、7-甲基香豆素、7-甲氧基香豆素），在10~120 μg/kg范围内不同加标水平下的平均回收率为70.8%~118.9%，相对标准偏差为0.19%~16.34%（n=6）。该法准确、灵敏、可靠，适用于玩具产品的实际检验工作和产品质量控制。

关键词: 超高效液相色谱-串联质谱, 儿童玩具, 液相微萃取, 致敏香豆素类化合物, 中空纤维膜

Abstract:

A comprehensive analytical method was developed for the determination of six allergenic coumarin compounds (coumarin, 7-methyl coumarin, 7-methoxycoumarin, 7-ethoxy-4-methyl coumarin, 4,6-dimethyl-8-tert-butyl coumarin and hexahydrocoumarin) in children's toys based on hollow-fiber liquid-phase microextraction (HF-LPME) followed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). HF-LPME was employed in sample pretreatment with the following parameters:extraction solvent of n-octanol, stirring rate of 700 r/min, extraction time of 50 min and amount of sodium chloride of 0.7 g. After chromatographic separation on an ACQUITY UPLC BEH Phenyl column (150 mm×2.1 mm, 1.7 μm), the target compounds were analyzed under multiple reaction monitoring (MRM) mode in positive electrospray ionization mode. The limits of quantification (LOQs) of the six allergenic coumarin compounds were either 2 μg/kg (7-ethoxy-4-methyl coumarin and 4,6-dimethyl-8-tert-butyl coumarin) or 10 μg/kg (coumarin, hexahydrocoumarin, 7-methyl coumarin and 7-methoxycoumarin). The average recoveries at different spiked levels ranged from 70.8% to 118.9% with relative standard deviations (RSDs) of 0.19%-16.34% (n=6). The proposed method is accurate, sensitive, reliable, and can be applied for the inspection and quality control of toy products.

Key words: allergenic coumarin compounds, children's toys, hollow-fiber membrane, liquid-phase microextraction (LPME), ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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