液相色谱-电感耦合等离子体质谱法测定水中铬形态  

Determination of chromium species in water by high performance liquid chromatography inductively coupled with plasma mass spectrometry

作　　者：郑晨阳 俞莎[1] 汤鋆[1] 谭莹[1] 马冰洁[1] 吴平谷[1] ZHENG Chen-yang;YU Sha;TANG Jun;TAN Ying;MA Bing-jie;WU Ping-gu(Zhejiang Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China)

机构地区：[1]浙江省疾病预防控制中心

出　　处：《中国卫生检验杂志》2019年第22期2707-2710,2714,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立液相色谱-电感耦合等离子体质谱法测定水中铬(Ⅲ)与铬(Ⅵ)的方法。方法采用动态反应池(Dynamic Reaction Cell,DRC)消除水体样品中碳和氯对铬ICP-MS测定的干扰,52Cr可作为铬形态分析的同位素。水样和铬形态标准溶液经复配络合剂络合,45℃放置10 min,采用DionexIonPac AS19(4 mm×250 mm)阴离子交换柱作为分析柱;以pH值=9.260 mmol/L硝酸铵溶液作为流动相,流速为1 ml/min。结果所建方法13 min内完成分析,铬(Ⅲ)与铬(Ⅵ)有很好的分离度,线性范围为1μg/L^50μg/L,线性相关系数r>0.9995,检出限分别为0.40μg/L和0.28μg/L;水中加标低、中、高3个浓度水平,加标回收率在90.8%~100.2%,相对标准偏差(RSD)分别为4.30%和2.38%。结论本方法灵敏度高、分析时间短、重现性及准确性好,适用于水体中铬形态的测定,为环境水体、饮用水及管材的安全监督检测提供切实可行的检测方法。Objective To develop a method for the determination of trivalent chromium and hexavalent chromium in water by high performance liquid chromatography-inductively coupled plasma mass spectrometry. Methods Dynamic reaction cell was used to reduce the polyatomic ion interferences of C and Cl in water to chromium determination by ICP-MS. 52Cr was suitable for chromium speciation analysis. The water sample solutions and the chromium species standard solutions were treated with mixed complexant to complex Cr under temperature of 45 ℃ for 10 min. Then, separation was performed on a DionexIonPac AS19(4 mm×250 mm) anion exchange column. 60 mmol/L ammonium nitrate(pH=9.2) was used as mobile phase with the flow rate of 1 ml/min. Results Separation and detection of Cr(Ⅲ) and Cr(Ⅵ) can be finished within 13 min. In the range of 1μg/L-50μg/L, the linear correlation coefficients(r) were greater than 0.999 5. The detection limits of the established method for Cr(Ⅲ) and Cr(Ⅵ) were 0.40 μg/L and 0.28 μg/L. Recoveries of low, medium, and high spiked levels were within 90.8%-100.2%. The relative standard deviations(RSDs) were 4.30% and 2.38%. Conclusion This method is sensitive, rapid, reproducible and accurate, and it is suitable for the determination of chromium species in water. The establishment of this method provides practical ways for supervision and detection of environmental water, drinking water and pipe safety.

关 键 词：液相色谱-电感耦合等离子体质谱法 水 铬形态 

分 类 号：R123.1[医药卫生—环境卫生学]