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人血清中18种全氟烷烃化合物UPLC-MS/MS的测定 [中文引用][英文引用]

Determination of 18 Perfluoroalkyl Substances in Human Serum by UPLC-MS/MS

作者:谢琳娜  张海婧  侯沙沙  朱英 
作者(英文):XIE Linna  ZHANG Haijing  HOU Shasha  ZHU Ying 
单位(英文): 
分类号:R113
出版年·卷·期(页码):2019·9·第5期(494-501)
DOI:
-----摘要:-------------------------------------------------------------------------------------------

目的 建立人体血清中18种全氟化合物的液液萃取超高效液相色谱串联质谱(UPLC-MS/MS)分析方法。方法 样品首先进行离子对液液萃取,经氮气吹干后,用甲醇复溶,最后用UPLC-MS/MS,在负离子条件下,采用多反应监测模式(MRM)进行分析检测。结果 18种全氟化合物在(0.01~5 ng/mL PFOS0.01~25 ng/mL)浓度范围内具有良好线性,相关系数(r)均大于0.998。该方法的检出限(LOD)在(0.01~0.1 ng/mL之间,定量限(LOQ)在(0.05~0.5 ng/mL之间。该方法的加标回收率良好,在71.4%~119.8%之间,平行样品间相对标准偏差小于15%。为验证方法的可靠性,采用四种国际认可的质控样品进行实验,结果与已有文献报道值和质控样品给出值相当。结论 该方法灵敏度高、重现性好、分析速度快,而且操作简便,可以实现对人体血清中18种全氟化合物的同时准确定量分析。

-----英文摘要:---------------------------------------------------------------------------------------

Objectives In order to develop a method for the simultaneous determination of 18 perfluoroalkyl substances in human serum samples, using ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-MS/MS). Methods Firstly, the human serum samples were extracted by ion-pair solution, and then concentrated to dryness under nitrogen. Secondly, the samples were redissolved with methanol and water. Finally, the extracts were quantified by UPLC-MS/MS. Results This method showed a good linear relationship from 0.01 to 5 ng/mL (PFOS is 0.01 to 25 ng/mL) of the 18 PFASs, and the correlation coefficients (r) is over 0.998. The limits of detection (LOD) were between 0.01 and 0.1 ng/mL, while the limits of quantitation (LOQ) were between 0.05 and 0.5 ng/mL. The recoveries of 18 PFASs were good, which were within 71.4%~119.8%, and the relative standard deviations between parallel samples were less than 15%. In order to verify the feasibility of this method, the experiment was conducted by four internationally recognized Quality Control Standards, of which the result were comparable with the reported and reference values. Conclusions The method is sensitive, repeatable, efficient and simple, which could be used for the precise quantitative analysis 18 PFASs in human serum samples.

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中文著录格式: 谢琳娜,,张海婧,,侯沙沙,,朱英.人血清中18种全氟烷烃化合物UPLC-MS/MS的测定.环境卫生学杂志.2019;9(5):494-501.
英文著录格式: XIE,Linna,,ZHANG,Haijing,,HOU,Shasha,,ZHU,Ying.Determination of 18 Perfluoroalkyl Substances in Human Serum by UPLC-MS/MS..2019;9(5):494-501.

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