摘要
本文建立了一种同位素内标稀释结合浓硫酸磺化处理,经液相色谱串联质谱对样品中五氯酚(Pentachlorophe-nol,PCP)及其钠盐快速分析筛查的方法.通过改变样品的pH值将样品中的五氯酚钠(Sodium pentachlorophenate,PCP-Na)转化成五氯酚后,用正己烷提取后辅以浓硫酸磺化,后采用高效液相色谱串联质谱法进行测定,内标法定量.结果显示,五氯酚在 0.15～10 ng/mL范围内线性关系良好,相关系数r＞0.999;方法加标试验的平均回收率为 90%～101%、RSD为4.17%～12.69%(n=6),检出限和定量限分别为0.15 μg/kg、0.50 μg/kg.结果表明,该方法操作简便,准确度和灵敏度较高,检出限、定量限均达到痕量分析标准,为五氯酚及其钠盐的快速检测提供了方法依据.
Abstract
A method was developed for the rapid analysis and screening of Pentachlorophenol(PCP)and its sodium salts in sam-ples by using liquid chromatography-tandem mass spectrometry(LC-MS)after internal standard dilution combined with concentrated sulfuric acid sulfonation.Sodium pentachlorophenate(PCP-Na)in the sample was converted into pentachlorophenate by changing the pH value of the sample,then extracted with n-hexane,sulfonated with concentrated sulfuric acid,determined by high performance liquid chromatography tandem mass spectrometry,and quantified by internal standard method.The results demonstrated that the linear relationship of pentachlorophenol was good in the range of 0.15-10 ng/mL,and the correlation coefficient r was＞0.999.The average recoveries from the spiking experiments were 90%to 101%,with an RSD of 4.17%to 12.69%(n=6).The limits of detection and quantitation were 0.15 μg/kg and 0.50 μg/kg,respectively.
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