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液相色谱-质谱法对饮用水中六价铬的测定
引用本文:王骏,胡梅,张卉,张喜琦,玄国东,祝建华.液相色谱-质谱法对饮用水中六价铬的测定[J].分析测试学报,2009,28(12).
作者姓名:王骏  胡梅  张卉  张喜琦  玄国东  祝建华
作者单位:山东省产品质量监督检验研究院,山东,济南,250100
摘    要:建立了液相色谱分离、电喷雾质谱测定饮用水中六价铬的方法.水样经微孔滤膜过滤后直接进样,以乙腈-1.5 mmol/L四丁基氢氧化铵水溶液为流动相,Xterra~(TM) MS C_(18)色谱柱分离六价铬,使用单四极杆质谱,选择离子模式检测,监测离子为m/z 118、117、101、85,其中117为定量离子.Cr(Ⅵ)的线性范围为1.0 ~100.0 μg/L,方法定量下限为1 μg/L.在空白水样中分别添加1.0、2.0、10.0 μg/L的六价铬,测得平均回收率(n=5)依次为91%、94%、97%,相对标准偏差分别为12.2%、7.4%、3.5%.测定了42个饮用水样品,其中17批检出六价铬,检出量为1.2 ~15.4 μg/L.

关 键 词:六价铬  饮用水  液相色谱-质谱

Determination of Hexavalent Chromium in Drinking Water by High Performance Liquid Chromatography-Mass Spectrometry
WANG Jun,HU Mei,ZHANG Hui,ZHANG Xi-qi,XUAN Guo-dong,ZHU Jian-hua.Determination of Hexavalent Chromium in Drinking Water by High Performance Liquid Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2009,28(12).
Authors:WANG Jun  HU Mei  ZHANG Hui  ZHANG Xi-qi  XUAN Guo-dong  ZHU Jian-hua
Abstract:A method for the determination of hexavalent chromium in drinking water by high performance liquid chromatography-electron-spray mass spectrometry was established.Sample was filtrated by a 0.45 μm micropore filter before injection.The separation of Cr(Ⅵ) was performed on a Xterra~(TM) MS C_(18) column using acetonitrile-1.5 mmol/L tetrabutyl ammonium hydroxide solution as mobile phase,and the detection of Cr(Ⅵ) was carried out under selected ion monitoring(SIM) mode with monitoring ions of m/z 118,117,101,85 and quantative ion of 117.The calibration curve of Cr(Ⅵ) was linear in the range of 1.0-100.0 μg/L with a quantitation limit of 1 μg/L.The avarge recoveries(n=5) of Cr(Ⅵ) from blank samples spiked with three levels of 1.0,2.0,10.0 μg/L were 91%,94%,97%,respectively,and the corresponding relative standard deviation were 12.2%,7.4%,3.5%,respectively.42 drinking water samples were used to test,and Cr(Ⅵ)was detected in 17 samples with the concentration of 1.2-15.4 μg/L.
Keywords:hexavalent chromium  drinking water  high performance liquid chromatography tandem mass spectrometry
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