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Chem. J. Chinese Universities ›› 2010, Vol. 31 ›› Issue (3): 473.

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Determination of Hexabromocyclododecane in Textiles by Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Qiang1*, BAI Hua1, WANG Chao1, XI Hai-Wei2, MA Wei3,4, ZHOU Xin1, DONG Yi-Yang1, WANG Bao-Lin1   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
    2. College of Chinese Pharmacy, Beijing University of Chinese Medicine, Beijing 100102, China;
    3. College of Food Science and Nutritional Engineering, China Agricultural University, Beijing 100083, China;
    4. Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150086, China
  • Received:2009-11-06 Online:2010-03-10 Published:2010-03-10
  • Contact: MA Qiang. E-mail: maqiang1129@yahoo.com.cn
  • Supported by:

    中国检验检疫科学研究院基本科研业务费专项资金资助.

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Abstract:

A comprehensive analytical method based on isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry has been developed for the determination of α-,β-,γ-hexabromocyclododecane in textiles. Various textile samples were extracted under 10.3 MPa and 80 ℃ by accelerated solvent extraction method with two static cycles using hexane-acetone(1∶1, volume ratio) as the extraction solvent. The reconstructed solution was then cleaned up by ENVI-CarbⅡ/PSA solid phase extraction cartridge. Qualitative and quantitative analysis was carried out for the analyte under the MRM mode after the chromatographic separation on Waters ACQUITY UPLC BEH phenyl(50 mm×2.1 mm, 1.7 μm) column with methanol-water gradient elution. The limit of quantitation(LOQs) for α-,β-,γ-hexabromocyclododecane was 0.5 μg/kg. The mean recoveries at the three spiked levels of 0.5—10 μg/kg were 84.2%—93.7%, with the intra-day precision less than 10% and the inter-day precision less than 12%. This method is accurate, rapid, sensitive and adapt to the inspection of hexabromocyclododecane in textiles.

Key words: Isotope dilution; Ultra performance liquid chromatography-tandem mass spectrometry; Textiles; Hexabromocyclododecane

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