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固相萃取-超高效液相色谱串联质谱法测定饮用水中11种全氟化合物

[Determination of 11 perfluorinated compounds in drinking water by solid phase extraction-ultra high performance liquid chromatography tandem mass spectrometry].

作者信息

Wen Xin, Lyu Jia, Chen Yongyan, Zhang Lan

机构信息

National Institute of Environmental Health, Chinese Center for Disease Control and Prevention, Beijing 100050, China.

出版信息

Wei Sheng Yan Jiu. 2020 Mar;49(2):272-279. doi: 10.19813/j.cnki.weishengyanjiu.2020.02.018.

Abstract

OBJECTIVE

To develop a method for the determination of 11 perfluorinated compounds(PFCs) in drinking water by solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).

METHODS

The target analytes in water samples were concentrated and purified by Oasis WAX SPE column and eluted with 5 mL methanol and 7 mL 0. 1% ammonia-methanol solution. The eluent was blown to near dryness under a nitrogen gas, diluting with methanol water solution(3∶7, V/V) to 1 mL for analysis by UPLC-MS/MS.

RESULTS

There were good liner relationship in the range of 0. 5-50 μg/L. The detection limit and the limit of quantitation were 0. 03-0. 7 ng/L and 0. 5-3. 0 ng/L, respectively. The recoveries of 11 PFCs at three different spiked concentrations were 90. 0%-122. 3%, 87. 1%-130. 0% and 80. 0%-113. 7%, respectively, and the relative standard deviation were 1. 95%-8. 59%, 1. 27%-9. 08% and 2. 17%-10. 51%(n=6), respectively.

CONCLUSION

This method has wide linear range, low detection limit and limit of quantitation, applicable for simultaneous analysis and monitorting of 11 PFCs in drinking water.

摘要

目的

建立一种固相萃取 - 超高效液相色谱串联质谱法(UPLC - MS/MS)测定饮用水中11种全氟化合物(PFCs)的方法。

方法

水样中的目标分析物经Oasis WAX固相萃取柱浓缩净化,用5 mL甲醇和7 mL 0.1%氨 - 甲醇溶液洗脱。洗脱液在氮气下吹至近干,用甲醇水溶液(3∶7,V/V)稀释至1 mL,供UPLC - MS/MS分析。

结果

在0.5 - 50 μg/L范围内线性关系良好。检出限和定量限分别为0.03 - 0.7 ng/L和0.5 - 3.0 ng/L。11种PFCs在3个不同加标浓度下的回收率分别为90.0% - 122.3%、87.1% - 130.0%和80.0% - 113.7%,相对标准偏差分别为1.95% - 8.59%、1.27% - 9.08%和2.17% - 10.51%(n = 6)。

结论

该方法线性范围宽,检出限和定量限低,适用于饮用水中11种PFCs的同时分析和监测。

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