建立了快速检测水产品中23种全氟烷基化合物(Perfluorinated alkyl substances,PFASs)的超快速液相色谱-串联质谱(UFLC-MS/MS)分析方法。样品前处理采用QuEChERS方法,以酸化乙腈提取目标物,C18填料和石墨化碳黑(GCB)分散固相萃取净化,C18色谱柱分离,甲醇和5 mmol/L乙酸铵溶液梯度洗脱,多反应监测负离子模式扫描。在最佳实验条件下,采用同位素标记的内标物进行内标法定量,以提高方法的准确度。23种目标物在12 min内实现良好分离,并在各自相应浓度范围内线性良好,相关系数不低于0.995,检出限为0.002~0.02μg/kg。加标回收率在75.6%~118.2%之间,相对标准偏差(RSD)为2.7%~14.5%。本方法操作简便,灵敏度高,适用于大批量样品的快速分析。
A method was proposed for the determination of 23 perfluorinated alkyl substances(PFASs) in fishery products by the QuEChERS method and ultra fast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS).The sample was extracted with acidified acetonitrile,cleaned-up by dispersive solid-phase extraction using C18 and graphitized carbon blacks(GCB).The separation of 23 PFASs was performed on a Kinetex XB-C18(100 mm×2.1 mm,2.6 μm) column using gradient elution of 5 mmol/L ammonium acetate and methanol as mobile phase within 12 min.The PFASs were analyzed under the multiple reaction monitoring(MRM) mode with negative electrospay ionization.Under the optimal conditions,the isotope internal standard method was used to determine the content of 23 PFASs,and improved the quantitative accuracy.The calibration curves were linear well with correlation coefficient over 0.995.The limits of detection ranged from 0.002 to 0.02 μg/kg.The average spiked recoveries for 23 PFASs were between 75.6% and 118.2%,with relative standard derivations(RSDs) from 2.7% to 14.5%.The developed method is simple and sensitive,and was suitable for rapid analysis of large quantities of samples.