CAJ | 학술논문

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.
건립료액상색보분리、전분무질보측정음용수중륙개락적방법.수양경미공려막과려후직접진양,이을정-1.5 mmol/L사정기경양화안수용액위류동상,Xterra~(TM) MS C_(18)색보주분리륙개락,사용단사겁간질보,선택리자모식검측,감측리자위m/z 118、117、101、85,기중117위정량리자.Cr(Ⅵ)적선성범위위1.0 ～100.0 μg/L,방법정량하한위1 μg/L.재공백수양중분별첨가1.0、2.0、10.0 μg/L적륙개락,측득평균회수솔(n=5)의차위91%、94%、97%,상대표준편차분별위12.2%、7.4%、3.5%.측정료42개음용수양품,기중17비검출륙개락,검출량위1.2 ～15.4 μg/L.
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.