Citation: XIE Lin-Na, ZHANG Hai-Jing, HOU Sha-Sha, ZHU Ying. Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Solid Phase Extraction for Determination of 15 Kinds of Perfluoroalkyl Acid[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(12): 1967-1972. doi: 10.19756/j.issn.0253-3820.191342 shu

Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Solid Phase Extraction for Determination of 15 Kinds of Perfluoroalkyl Acid

National Institute of Environmental Health, Chinese Center for Disease Control and Prevention, Beijing 100021, China

Received Date: 19 June 2019
Revised Date: 5 November 2019

Fund Project: This work was supported by the National Program for Central Financial Funds of China-Construction of Human Biomonitoring System for Environmental Pollution (No. 131031108000150003).

A method was established for simultaneous determination of 15 kinds of perfluoroalkyl carboxylic acids (PFCAs) and perfluoroalkane sulfonic acids (PFSAs) in soil sample using ultra performance liquid chromatography-tandem mass spectrometry coupled with solid phase extraction (SPE-UPLC-MS/MS). Firstly, 1 g of soil sample was ultraphonic extracted and then purified by SPE cartridge. The extracts were finally quantified by UPLC-MS/MS in negative electrospray ionization and multiple reaction monitoring (MRM) mode. The solvent volume and time of sonicated extraction, and the method of solid-phase extraction were optimized, and a satisfied pre-treatment effect was achieved when the sample was treated by ultraphonic extraction for 15 minutes in 2 mL of 1% ammonium hydroxide/methanol solution and eluted by methanol and 0.1% ammonium hydroxide/methanol successively on ENVI-Carb SPE cartridges. This method showed a good linear relationship in the concentration range of 0.01-5 ng/mL for the 15 kinds of PFCAs and PFSAs (R>0.998). The limits of detection (LOD) were in the range of 0.002-0.016 ng/g, while the limits of quantitation (LOQ) were in the range of 0.006-0.050 ng/g. The recoveries were 75.8%-113.0%, with relative standard deviations (RSDs) of less than 15%. Compared with the reported methods, comparable or even better quantification results were obtained by the method. The internationally accredited quality control sample NIST SRM 2586 was measured, and it was in the range of given concentration, which meant that this method was feasible for determination of PFAAs. Compared with the reported methods, this method consumed less solvent with shorter pretreatment time, and could be used for accurate analysis of PFAAs in soil.
- Perfluoroalkyl acids,
- Soil,
- Solid phase extraction,
- Ultrasonic extraction,
- , Ultra performance liquid chromatography-tandem mass spectrometry
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