自动复合硅胶柱净化-气相色谱串联质谱法测定饲料中多氯联苯

Determination of polychlorinated biphenyls in feedstuffs by automated composite silica gel column clean-up coupled with gas chromatography-tandem mass spectrometry

本实验基于自动复合硅胶柱前处理结合气相色谱串联质谱技术,旨在建立同时检测饲料及饲料原料中7种指示性多氯联苯(IN-PCBs)的方法。样品中的IN-PCBs经溶剂加速萃取后,采用复合硅胶净化柱正压自动净化处理,应用岛津GCMS TQ8050三重四级气质联用仪检测,同位素稀释法定量。结果表明:标准曲线线性范围0.1~100 ng/mL,相关系数(R 2)均大于0.999,平均相对响应因子为0.91~1.14;检测限为0.6~8.2 ng/kg,平均加标回收率为88.1%~108.4%,相对标准偏差为1.0%~13.0%。与传统方法相比,本方法前处理时间短、检测灵敏度高,能够满足饲料及相关产品中IN-PCBs监测与风险评估的需求。

A method was developed for the determination of seven indicator polychlorinated biphenyls(IN-PCBs)in feedstuffs by automated clean-up coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS).The analytical procedure consisted of accelerated solvent extraction,decontamination with composite silica gel column,detection with GC-MS/MS and isotope dilution method for quantification.The results showed that the calibration curves with good correlation coefficients(R 2>0.999)were obtained in the concentration range of 0.1~100 ng/mL.The average relative response factors of IN-PCBs were 0.91~1.14,and the limit of detection was 0.6~8.2 ng/kg.The average recoveries of IN-PCBs in feedstuffs at three spiked concentration levels ranged from 88.1%to 108.4%with relative standard deviations between 1.0%~13.0%(n=5).Compared to conventional methods,the present method has a short pre-treatment time and high detection sensitivity and could meet the needs of monitoring and risk assessment of IN-PCBs in feed and related products.