液相色谱-电感耦合等离子体质谱法同时测定尿液中6种砷形态  

Simultaneous determination of six arsenic species in urine using liquid chromatography-inductively coupled plasma mass spectrometry

作　　者：张春华[1] 陈亮[1] 陈春桃 韩必恺 朱志鑫[1] 吴惠勤[1] 黄晓兰[1] ZHANG Chun-hua;CHEN Liang;CHEN Chun-tao;HAN Bi-kai;ZHU Zhi-xin;WU Hui-qin;HUANG Xiao-lan(Guangdong Provincial Public Laboratory of Analysis and Testing Technology, China National Analytical Center ( Guangzhou) , Guangzhou 510070, China)

机构地区：[1]中国广州分析测试中心广东省分析测试技术公共实验室

出　　处：《分析试验室》2019年第6期709-712,共4页Chinese Journal of Analysis Laboratory

摘　　要：建立了HPLC-ICP-MS测定尿液中6种砷形态的方法。直接过滤或是纯水稀释后过滤处理样品,以20 mmol/L NH4H2PO4(pH 8. 0)作为流动相,Hamilton PRP-X100 (250 mm×4. 1 mm,10μm)阴离子交换分析柱分离砷胆碱(AsC),砷甜菜碱(AsB),As(Ⅲ),二甲基砷(DMA),一甲基砷(MMA)和As(Ⅴ),ICP-MS测定6种形态砷。在优化的测试条件下,6种形态砷在0. 5~100μg/L或1~100μg/L范围内线性关系良好,相关系数均大于0. 9998。在低、中、高3个加标浓度水平,6种形态砷的回收率为87. 0%~109. 3%,平均回收率为89. 6%~108. 0%,RSD为0. 65%~4. 3%。AsC,AsB,As(Ⅲ),DM A,M M A和As(Ⅴ)的检出限分别为0. 4,0. 3,0. 4,0. 4,0. 3,0. 5μg/L。方法可用于正常人尿液、砷中毒患者尿液或是接受砷剂治疗的白血病患者的尿液中砷形态的测定。A new method has been established for the rapid and simultaneous analysis of six arsenic species included As C,As B,As( Ⅲ),DMA,MMA and As( Ⅴ) in urine. The urine sample was pretreated through direct membrane filtering,or dilution filtering. Six arsenic species were separated through a Hamilton PRP-X100( 250 mm × 4. 1 mm,10 μm) anion exchange column with 20 mmol/L NH4 H2 PO4( pH 8. 0) as mobile phase,and then detected by inductively coupled plasma mass spectrometry( ICP-MS). Under the optimum conditions,the calibration curves of the six arsenic species are linear over a range of 0. 5-100 μg/L or 1-100 μg/L in urine,and the correlation coefficients( R^2) are higher than 0. 9998. At the low,middle and high spiked levels,the recoveries and average recoveries for the six arsenic compounds ranged from 87. 0% to 109. 3% and 89. 6% to108. 0%,respectively. The relative standard deviations( RSDs) are 0. 65%-4. 3%. The limits of detection for As C,As B,As( Ⅲ),DMA,MMA and As( Ⅴ) are 0. 4,0. 3,0. 4,0. 4,0. 3 and0. 5 μg/L,respectively. The method, proved as rapid and easy to handle, is suitable for the simultaneous determination of the six arsenic species in urine samples of poisonous patients or leukemia patients who received arsenical treatment.

关 键 词：液相色谱-电感耦合等离子体质谱法 砷形态 尿液 

分 类 号：R446[医药卫生—诊断学]