分散固相萃取结合稳定同位素内标-气相色谱-串联质谱法快速测定牛奶中7种多溴二苯醚
Chinese Journal of Food Hygiene(2020)
Abstract
目的 建立同时测定牛奶中7种多溴二苯醚(PBDEs)的分散固相萃取结合13C稳定同位素内标-气相色谱-串联质谱(GC-MS/MS)法.方法 样品添加13C12同位素内标后,以1%乙酸乙腈提取,采用新型Z-Sep+C18为吸附剂净化,DB-5色谱柱(30 m×0.25 mm,0.25μm)分离,选择电子轰击源(EI)多反应监测模式(MRM)气相色谱-串联质谱进行测定,基质匹配标准曲线同位素内标法定量.结果 7种PBDEs在0.500~100 ng/mL范围内均呈良好的线性关系,相关系数r均大于0.999;在0.1、1.0、10μg/kg 3个加标水平下的平均回收率为89.7%~102.9%,相对标准偏差(n=6)为3.8%~8.3%;检出限和定量下限分别为2.4~9.8和7.5~30 ng/kg.结论 该方法简单、快速、重现性好、灵敏度高,可满足牛奶中7种多溴二苯醚的检测要求.
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Key words
gas chromatography-tandem mass spectrometry,isotope labeled internal standard,dispersive solid phase extraction,polybrominated diphenyl ethers,milk
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