论文部分内容阅读
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 method for PFOA and PFOS and its typical isoforms for serum pre-treatment to develop simple and efficient ultra-high performance liquid of PFOA and PFOS and its typical isomers Phase chromatography-tandem mass spectrometry (UPLC-MS / MS) analysis provides the basis for the large-scale monitoring of typical perfluorochemical isomers in human serum matrices. Methods The samples were diluted with 4% phosphoric acid and directly concentrated on weak anion solid phase extraction (SPE) column. The target compounds were concentrated by HSS PFP column, ESI negative ion source and MRM (Multiple Reaction Monitoring Mode) Internal standard method. Results The recoveries of 16 isomers were 80.1% ~ 115.6% with relative standard deviations of 0.8% ~ 12.7%. The 16 isoforms in serum had a good linear relationship (r> 0.999) in their respective linear ranges with a detection limit of 2 pg / ml to 100 pg / ml. Conclusion The method is simple, rapid and sensitive. It can meet the detection requirements of perfluorooctanoic acid and perfluorooctane sulfonate in serum and its typical isomers.