高效液相色谱–串联质谱法检测环境水体中18种全氟化合物

Determination of 18 perfluorinated alkyl substances in environmental water by high performance liquid chromatography–tandem mass spectrometry

建立了快速检测环境水体中18种全氟化合物的高效液相-串联质谱方法。环境水样经大体积PEP固相萃取柱快速提取、富集和净化后,过0.22μm微孔滤膜,再利用Agilent Zorbax Eclipse XDB-C18反相色谱柱分离,以5 mmol/L乙酸铵溶液和甲醇为流动相梯度洗脱,最终进入电喷雾离子源负离子扫描,在多反应监测模式下定性及定量分析。所有目标化合物的质量浓度在1~20μg/L范围内与色谱峰面积线性良好,相关系数(r2)大于0.999,方法检出限为0.18~0.48 ng/L。18种全氟化合物的加标回收率为90.1%~107.3%,相对标准偏差为0.3%~8.2%(n=6)。该方法操作简单、快速,灵敏度高,可满足环境水体中全氟化合物的检测。

A method was established for the determination of 18 perfluorinated alkyl substances(PFASs)in environmental water by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The environmental water sample was quickly extracted,enriched and cleaned-up by PEP solid phase extraction,then filtered through 0.22μm microporous membrane;the separation of 18 PFASs was performed on an Agilent Zorbax Eclipse XDB-C18 column using gradient elution of 5 mmol/L ammonium acetate and methanol as mobile phase.PFASs were analyzed under the multiple reaction monitoring(MRM)mode with negative electrospay ionization.The calibration curves of all PFASs had a good linear relationship with the chromatographic peak area in the range of 1-20μg/L with the correlation coefficients(r2)more than 0.999.The detection limits ranged from 0.18 ng/L to 0.48 ng/L.The spiked recoveries for 18 PFASs were between 90.1%and 107.3%with the relative standard derivations from 0.3%to 8.2%(n=6).The developed method is simple,rapid and sensitive,and it is suitable for rapid analysis of PFASs in environmental water.