水溶剂加速萃取-超高效液相色谱串联质谱测定土壤中全氟羧酸

罗火焰; 宋洲; 皮施施; 吉义平; 周宇齐; 杨杰

引用本文:	LUO Huoyan,SONG Zhou,PI Shishi,JI Yiping,ZHOU Yuqi,YANG Jie.Determination of Perfluorinated Carboxylic Acids in Soil by Accelerated Aqueous Solvent Extraction Coupled with Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry[J].Environmental Monitoring and Forewarning,2024,(2):66~72

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水溶剂加速萃取-超高效液相色谱串联质谱测定土壤中全氟羧酸
罗火焰^1,2，宋洲^3,4*，皮施施¹，吉义平³，周宇齐³，杨杰³
1.湖北华祥地质环境检测科技有限公司，湖北武汉 430000；2.中国地质大学（武汉），湖北武汉 430074；3.湖北省地质实验测试中心，湖北武汉 430034；4.资源与生态环境地质湖北省重点实验室（湖北省地质局），湖北武汉 430034

摘要:

采用水溶剂加速萃取-超高效液相色谱串联质谱法（UPLC-MS/MS）建立了土壤中6种全氟羧酸（PFCs）的分析方法，并对色谱分析条件、水溶剂萃取条件、固相萃取柱净化条件及实验材料选择等进行了优化。结果表明，以ACQUITY UPLC BEH C18色谱柱为分离柱，2.0 mmol/L乙酸铵水溶液为流动相A，甲醇为流动相B，梯度洗脱下可在9 min内完成6种PFCs的测试，检出限为0.03~0.4 μg/kg。对实际土壤样品进行测定，加标回收率为90.7%~118%，相对标准偏差为5.6%~18.0%，精密度和准确度均较好。该方法前处理过程简单、易操作，仪器检测效率高、结果准确，能够满足土壤中PFCs的检测要求。

关键词: 全氟羧酸土壤水加速溶剂萃取超高效液相色谱串联质谱法

DOI：DOI：10.3969/j.issn.1674-6732.2024.02.010

分类号:X833

基金项目:湖北省地质局科研项目（KJ2020-30，KJ2022-36）

Determination of Perfluorinated Carboxylic Acids in Soil by Accelerated Aqueous Solvent Extraction Coupled with Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

LUO Huoyan^1,2， SONG Zhou^3,4*， PI Shishi¹， JI Yiping³， ZHOU Yuqi³， YANG Jie³

1. Hubei Huaxiang Geological Environment Testing Technology Co.， Ltd.， Wuhan， Hubei 430000， China；2.China University of Geosciences（Wuhan）， Wuhan，Hubei 430074， China；3.Hubei Province Geological Experimental Testing Center，Wuhan，Hubei 430034， China； 4.Hubei Key Laboratory of Resources and Eco environment Geology（Hubei Geological Bureau）， Wuhan， Hubei 430034， China

Abstract:

An analytical method for the determination of six perfluorocarboxylic acids(PFCs) in soil was established by accelerated aqueous solvent extraction coupled with ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)， and the chromatographic conditions， aqueous solvent extraction conditions， solid phase extraction column clean up conditions and the selection of experimental materials were optimized. The results showed that the six PFCs could be analyzed on an ACQUITY UPLC BEH C18 column with 2.0 mmol/L methanol ammonium acetate aqueous solution as the mobile phase in a gradient elution mode in 9 min， and the limits of detection(LODs) were in the range of 0.03～0.4 μg/kg. The recoveries of the spiked PFCs for the determination of the actual soil samples were in the range of 90.7 %～118 %， and the relative standard deviations(RSD) were 5.6 %～18.0 %， which showed good precision and accuracy. The method is simple and easy to operate， and the instrumental detection efficiency is high with accurate results， which can meet the requirements for the determination of PFCs in soil.

Key words: Perfluorocarboxylic acid Soil Aqueous Accelerated solvent extraction Ultra high performance liquid chromatography tandem mass spectrometry