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

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

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0.03~0.4μg/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。

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 0.03~0.4μg/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.