超高效液相色谱-串联质谱法测定血清中的全氟辛酸和全氟辛烷磺酸及其典型异构体  被引量:8

Simultaneous determination of perfluorooctanoate,perfluorooctane sulfonate and its typical isomers in serum by ultra performance liquid chromatography-tandem mass spectrometry

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作  者:谢丹 王雨昕 李敬光[2,3] 赵云峰 吴永宁[2,3] 

机构地区:[1]武汉轻工大学食品科学与工程学院,湖北武汉430023 [2]国家食品安全风险评估中心,北京100022 [3]卫生部食品安全风险评估重点实验室,北京100022

出  处:《中国卫生检验杂志》2017年第19期2737-2741,共5页Chinese Journal of Health Laboratory Technology

基  金:国家自然科学基金重点项目(21537001)

摘  要:目的建立灵敏和准确可靠的全氟辛酸和全氟辛烷磺酸及其典型同分异构体血清前处理方法,开发简单高效的全氟辛酸和全氟辛烷磺酸及其典型异构体的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,为大规模监测人体血清基质中的典型全氟化合物同分异构体奠定基础。方法样品经4%磷酸稀释后直接过弱阴离子固相萃取柱对样品中目标化合物进行富集浓缩,经HSS PFP柱分离,采用ESI负离子源并在多反应监测模式(MRM)下进行测定,同位素内标法定量。结果 16种同分异构体的回收率为80.1%~115.6%,相对标准偏差为0.8%~12.7%。血清中16种同分异构体在各自的线性范围内线性关系良好(r>0.999),检出限在2 pg/ml^100 pg/ml。结论本方法简便、快速,且灵敏度高,可以满足血清中全氟辛酸和全氟辛烷磺酸及其典型异构体的检测需求。Objective To establish a sensitive and accurate pre-treatment method for perfluorooctanoic acid,perfluorooctane sulfonate and its typical isomers in serum,to develop a simple and efficient ultra-high performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) for perfluorooctanoic acid,perfluorooctane sulfonate and its typical isomers,so as to build up the foundation for large-scale detection of typical perfluorinated compound isomers in human serum.Methods The sample was enriched and cleaned up with WAX solid phase extraction column after diluted with 4% phosphoric acid,then separated on HSS PFP column and finally detected by UPLC-MS/MS in negative ionization and multiple reaction monitoring mode. Results The average recoveries of sixteen isomers were within 80. 1%-115. 6%,with the relative standard deviations( RSDs) of 0. 8%-12. 7%. This method showed a good liner relationship with the correlation coefficients( r) over0. 999. The detection limits of sixteen compounds in serum were within 2 pg/ml-100 pg/ml. Conclusion This method is simple,rapid,sensitive,and it can be used for the detection of perfluorooctanoate,perfluorooctane sulfonate and its typical isomers in serum.

关 键 词:全氟辛烷磺酸 全氟辛酸 血清 超高效液相色谱-串联质谱法 

分 类 号:O657.63[理学—分析化学]

 

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