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

Previous Articles     Next Articles

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).

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)

CLC Number: