RPIP-HPLC-ICP-MS测定饮用水中铬形态
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摘要
本文建立一种改进的高效液相色谱-电感耦合等离子体质谱法测定淡水中铬形态的方法。通过样品加标回收验证本方法的准确度,本方法 Cr(Ⅲ)和Cr(Ⅵ)的回收率均在93%~115%之间。通过制备7个浓度水平确定得到铬元素的校准曲线范围,Cr(Ⅲ)和Cr(Ⅵ)的相关系数接近1(r=0.999 9),Cr(Ⅲ)和Cr(Ⅵ)的LOD分别为0.094、0.100μg/L,Cr(Ⅲ)的LOQ为0.28μg/L,Cr(Ⅵ)为0.30μg/L。综上所述,方法的定量限、重现性和准确度满足淡水中Cr(Ⅲ)和Cr(Ⅵ)的定量分析,可以有效应用于其预期的使用。
The approach presented in this paper refered to the modification of a method for the detection and quantitative determination of chromium species in water by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The accuracy of the method was verified by sample adding recovery estimation. The recovery rates of both determined analytes were between 93% and 115%.Calibration curve was obtained by preparing seven concentration levels of each chromium species. In both cases,the correlation coefficient was close to 1(r=0.999 9)for Cr(Ⅲ)and Cr(Ⅵ). Using the HPLC-ICP-MS method,LOD was 0.094 μg/L and 0.100 μg/L for Cr(Ⅲ)and Cr(Ⅵ),respectively. According to the modified blank determination method,LOQ for Cr(Ⅲ)was 0.28 μg/L and for Cr(Ⅵ)was 0.30 μg/L.As a result of the method validation experiment,the obtained limit of quantification,repeatability and intermediate precision were satisfied for the quantification of Cr(Ⅲ)and Cr(Ⅵ)in water matrices. The method can be applied effectively for its intended use.
The approach presented in this paper refered to the modification of a method for the detection and quantitative determination of chromium species in water by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The accuracy of the method was verified by sample adding recovery estimation. The recovery rates of both determined analytes were between 93% and 115%.Calibration curve was obtained by preparing seven concentration levels of each chromium species. In both cases,the correlation coefficient was close to 1(r=0.999 9)for Cr(Ⅲ)and Cr(Ⅵ). Using the HPLC-ICP-MS method,LOD was 0.094 μg/L and 0.100 μg/L for Cr(Ⅲ)and Cr(Ⅵ),respectively. According to the modified blank determination method,LOQ for Cr(Ⅲ)was 0.28 μg/L and for Cr(Ⅵ)was 0.30 μg/L.As a result of the method validation experiment,the obtained limit of quantification,repeatability and intermediate precision were satisfied for the quantification of Cr(Ⅲ)and Cr(Ⅵ)in water matrices. The method can be applied effectively for its intended use.
引文
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[16]VANHAECKE F,SAVERWYNS S,DE WANNEMACKER G,et al.Comparison of the application of higher mass resolution and cool plasma conditions to avoid spectral interferences in Cr(III)/Cr(VI)speciation by means of high-performance liquid chromatography-inductively coupled plasma mass spectrometry[J].Anal Chim Acta,2000(419):55-64.
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[18]XIE Q,KERRICH R,IRVING E,et al.Determination of five arsenic species in aqueous samples by HPLC coupled with a hexapole collision cell ICP-MS[J].J Anal At Spectrom,2002(17):1037-1041.
[19]CASTILLO A,ROIG-NAVARRO A F,POZO O J.Capabilities of microbore columns coupled to inductively coupled plasma mass spectrometry in speciation of arsenic and selenium[J].J Chromatogr A,2008(1202):132-137.
[2]METZE D,JAKUBOWSKI N,KLOCKOW D.Speciation of chromium[M]//CORNELIS R,CREWS H,CARUSO J,et al.Handbook of elemental speciation II:Species in the environment,food,medicine and occupational health.New York:Wiley,2005.
[3]WROBEL K,CARUSO JA.Elemental and isotope ratio mass spectrometry[M]//GROSS M L,CAPRIOLI R M.The encyclopedia of mass spectrometry,Volume 5:elemental and isotope ratio mass spectrometry.Oxford:Elsevier,2010.
[4]EIDEN G,BARINAGA C J,KOPPENAAL D W[M]//GROSS ML,CAPRIOLI RM.The encyclopedia of mass spectrometry,Volume 5:elemental and isotope ratio mass spectrometry.Oxford:Elsevier,2010.
[5]KONIECZKA P,NAMIES′NIK J.Quality assurance and quality control in the analytical chemical laboratory[M]//A practical approach.Boca Raton:Taylor&Francis Group,2009.
[6]KUO CY,JIANG SJ,SAHAYAM AC.Speciation of chromium and vanadium in environmental samples using HPLC-DRC-ICP-MS[J].J Anal At Spectrom,2007(22):636-641.
[7]CHANG Y L,JIANG S J.Determination of chromium species in water samples by liquid chromatography-inductively coupled plasma-dynamic reaction cell-mass spectrometry[J].J Anal At Spectrom,2001(16):858-862.
[8]NEUBAUER K,REUTER W,PERRONE P.Chromium speciation in water by HPLC/ICP-MS:Application Note[Z].Norwalk:Perkin Elmer,2003.
[9]EURACHEM GUIDE.The fitness for purpose of analytical methods:a laboratory guide to method validation and related topics[Z].Teddington:LGC,1998.
[10]GURLEYUKH,WALLSCHLA¨GERD.Determination of chromium(III)and chromium(VI)using suppressed ion chromatography inductively coupled plasma mass spectrometry[J].J Anal At Spectrom,2001(16):926-930.
[11]XING L,BEAUCHEMIN D.Chromium speciation at trace level in potable water using hyphenated ion exchange chromatography and inductively coupled plasma mass spectrometry with collision/reaction interface[J].J Anal At Spectrom,2010(25):1046-1055.
[12]International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use.ICH Guideline Q2(R1):validation of analytical procedures:text and methodology[EB/OL].[2013-02-12].http://www.ich.org/.
[13]CHEN Z L,MEGHARAJ M,NAIDU R.Removal of interferences in the speciation of chromium using an octopole reaction system in ion chromatography with inductively coupled plasma mass spectrometry[J].Talanta,2007(73):948-952.
[14]WOLF R E,MORRISON J M,GOLDHABER M B.Simultaneous determination of Cr(III)and Cr(VI)using reversed-phased ionpairing liquid chromatography with dynamic reaction cell inductively coupled plasma mass spectrometry[J].J Anal At Spectrom,2007(22):1051-1060.
[15]WANG HJ,DU XM,WANG M,et al.Using ion-pair reversed-phase HPLC ICP-MS to simultaneously determine Cr(III)and Cr(VI)in urine of chromate workers[J].Talanta,2010(81):1856-1860.
[16]VANHAECKE F,SAVERWYNS S,DE WANNEMACKER G,et al.Comparison of the application of higher mass resolution and cool plasma conditions to avoid spectral interferences in Cr(III)/Cr(VI)speciation by means of high-performance liquid chromatography-inductively coupled plasma mass spectrometry[J].Anal Chim Acta,2000(419):55-64.
[17]SE′BY F,CHARLES S,GAGEAN M,et al.Chromium speciation by hyphenation of high-performance liquid chromatography to inductively coupled plasma-massspectrometry:study of the influence of interfering ions[J].J Anal At Spectrom,2003(18):1386-1390.
[18]XIE Q,KERRICH R,IRVING E,et al.Determination of five arsenic species in aqueous samples by HPLC coupled with a hexapole collision cell ICP-MS[J].J Anal At Spectrom,2002(17):1037-1041.
[19]CASTILLO A,ROIG-NAVARRO A F,POZO O J.Capabilities of microbore columns coupled to inductively coupled plasma mass spectrometry in speciation of arsenic and selenium[J].J Chromatogr A,2008(1202):132-137.