Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (02): 160-164.DOI: 10.3724/SP.J.1123.2011.10001

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Determination of five coumarins in toys by high performance liquid chromatography-tandem mass spectrometry

YANG Rongjing*, WEI Biwen, GAO Huan, YU Wenjia   

  1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2011-10-07 Revised:2011-11-14 Online:2012-02-28 Published:2012-03-22

Abstract: A rapid analytical method for the determination of five coumarins (coumarin, 7-methoxycoumarin, dihydrocoumarin, 7-methyl coumarin and 7-ethoxy-4-methyl coumarin) in toys by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed. After ultrasonic extraction in tetrahydrofuran, the samples were analyzed by HPLC-MS/MS in multi-reaction monitoring (MRM) mode. Acetonitrile and 0.1% acetic acid were used as the mobile phases with gradient elution. The linear ranges of calibration curves were 10~1000 μg/L, and the limits of quantification (LOQ) (S/N>10) were 2.0 μg/L for all the analytes, except that the LOQ for dihydrocoumarin was 5.0 μg/L. The recoveries of the five coumarins spiked in three types of samples were in the ranges of 93.2%~105.8%, 97.3%~ 103.2% and 96.8%~102.9%, with the relative standard deviations in the ranges of 4.35%~8.27%, 3.65%~6.73% and 4.03%~6.45%, respectively. The method was applied in the determination of 12 toy samples. The five analytes were found in 9 samples, and in some cases, the presence of quite high concentrations of these coumarins in the toys should be a matter of concern.

Key words: coumarins, fragrance allergens, toys, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)