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

A comprehensive analytical method based on isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry has been developed for the determination of alpha-, beta-, gamma-hexabromocyclododecane in textiles. Various textile samples were extracted under 10.3 MPa and 80 degrees C 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-Carb II/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 x 2.1 mm, 1.7 mu m) column with methanol-water gradient elution. The limit of quantitation (LOQs) for alpha-, beta-, gamma-hexabromocyclododecane was 0.5 mu g/kg. The mean recoveries at the three spiked levels of 0.5-10 mu g/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.