同位素内标稀释-分散固相萃取-液相色谱串联质谱测定环境水中五氯酚

Determination of pentachlorophenol in water by isotopo internal standard dilution-dispersive solid phase extraction-liquid chromatography coupled with tandem mss spectrometry

目的建立环境水样中五氯酚的同位素内标稀释-分散固相萃取-液相色谱串联质谱法的分析方法。方法环境水样用聚酰胺粉吸附、浓缩,1%甲酸甲醇(V/V)洗脱后分析。串联质谱在电喷雾(ESI)离子多反应监测(MRM)模式下检测目标化合物,以保留时间以及特征离子对进行定性,同位素内标法定量。结果五氯酚在0.5μg/L^50.0μg/L浓度内呈现良好的线性关系。五氯酚的方法检出限为0.003μg/L,定量限为0.01μg/L。平均回收率在92.5%~105.0%,相对标准偏差(RSD)为1.0%~2.7%。结论方法快速高效、灵敏度高、稳定性好,可用于环境水样中痕量五氯酚的监管监测。

Objective A method based on isotopo internal standard dilution-dispersive solid phase extraction-liquid chromatography coupled with tandem mass spectrometry has been developed for the determination of pentachlorophenol in water.Methods The sample was adsorbed and enriched by polyamide powder,and eluted by methanol(formia acid,1%,V/V).The analyte was determined by an electrospray ionization-mass spectrometry in multiple reaction monitoring(MRM)mode.The qualitative analyses were based on the retention time and characteristic ion pairs of the analyte.The quantitative analyse was internal standard method.Results Linearity for pentachlorophenol was in the range of 0.5μg/L-50.0μg/L.The limit of quantification(LOQ)was 0.01μg/L and the average recovery was in the range of 92.5%-105.0%with the relative standard deviations of 1.0%-2.7%.Conclusion The developed method is fast and efficient,sensitive,reproducible,and adapts to the routine analyses for the determination of pentachlorophenol in water samples.