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Citation: HU Mingzhu, LIAN Xianhui, LIU Han, GUO Xiangyu, LÜ Yueguang, BAI Hua, XUE Hongyu, MA Qiang. 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[J]. Chinese Journal of Chromatography, ;2017, 35(11): 1145-1151. doi: 10.3724/SP.J.1123.2017.08011 shu

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 Mingzhu ^1, ,
LIAN Xianhui ^1,2 ,
LIU Han ¹ ,
GUO Xiangyu ¹ ,
LÜ Yueguang ^1,3 ,
BAI Hua ¹ ,
XUE Hongyu ² ,
MA Qiang 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 Date: 16 August 2017

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

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.
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