同位素稀释-超高效液相色谱-串联质谱法测定纺织品中的六溴环十二烷

建立了同时测定纺织品中α-,β-,γ-六溴环十二烷的同位素稀释-超高效液相色谱-串联质谱分析方法.不同类型的纺织品样品采用加速溶剂萃取法,以正己烷-丙酮(体积比1∶1)混合液为萃取溶剂,在10.3 MPa和80℃下,静态循环萃取3次,每次5 min,萃取液经ENVI-CarbⅡ/PSA固相萃取柱净化,收集二氯甲烷-正己烷(体积比2∶3)洗脱液,采用Waters ACQUITY UPLC BEHPhenyl色谱柱(50 mm×2.1 mm,1.7μm),以甲醇-水为流动相梯度洗脱分离后进行UPLC/MS/MS多反应监测模式下的定性及定量分析.结果表明,α-,β-,γ-六溴环十二烷测定方法的定量限为0.5μg/kg,在0.5~10μg/kg浓度范围内,低、中及高3个添加水平的平均回收率为84.2%~93.7%,日内精密度均小于10%,日间精密度均小于12%.本方法准确快速,且灵敏度高,可用于纺织品的实际检验.

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 α-,β-,γ-hexabromocyclododecane in textiles. Various textile samples were extracted under 10.3 MPa and 80 ℃ by accelerated solvent 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.