高效液相色谱-电感耦合等离子体质谱法测定人尿中6种砷形态化合物  

Determination of six arsenic species in human urine by HPLC-ICP-MS

作　　者：何易 刘兰侠[2] 薛黎明[1] 熊丽蓓[1] 方亚敏[1] HE Yi;LIU Lanxia;XUE Liming;XIONG Libei;FANG Yamin(Shanghai Municipal Center for Disease Control and Prevention,Shanghai 200336,China;Xuhui Center for Disease Control and Prevention,Shanghai 200237,China)

机构地区：[1]上海市疾病预防控制中心,上海200336 [2]上海市徐汇区疾病预防控制中心,上海200237

出　　处：《上海预防医学》2023年第2期182-186,共5页Shanghai Journal of Preventive Medicine

基　　金：上海市自然科学基金项目(21ZR1454600);上海市卫生健康委员会重点项目(2020YZ001);上海市医苑新星青年医学人才培养资助计划(沪卫人事〔2021〕99号);国家环境保护新型污染物环境健康影响评价重点实验室建设项目(环科财函〔2020〕99号)。

摘　　要：【目的】建立高效液相色谱-电感耦合等离子体质谱(HPLC⁃ICP⁃MS)测定人尿中砷胆碱(AsC)、砷甜菜碱(AsB)、三价砷(As^(3+))、二甲基砷酸(DMA5+)、甲基砷酸(MMA5+)、五价砷(As^(5+))等6种砷形态化合物含量的方法。【方法】优化流动相pH值及无水乙醇含量,以50 mmol·L^(-1)的(NH4)2CO3溶液(含2%无水乙醇、pH=8.5)为流动相,用He模式消除氯离子(Cl-)干扰,通过Hamilton PRP X⁃100阴离子交换色谱柱对10倍稀释的人尿砷形态化合物进行分离,与ICP⁃MS联用,建立6种砷形态化合物的检测方法。【结果】6种砷形态化合物13 min左右可以得到完全分离,标准曲线线性相关系数为0.999,检出限为0.10~0.20μg·L^(-1),定量限为0.30~0.50μg·L^(-1)。精密度实验显示,加标浓度0.20μg·L^(-1)时相对标准偏差(RSD)为5.96%~9.07%;加标浓度2.00μg·L^(-1)时RSD为2.48%~6.38%,加标浓度5.00μg·L^(-1)时RSD为1.41%~2.57%。准确度实验显示,加标回收率为80%~125%。【结论】所建立HPLC⁃ICP⁃MS测定人尿6种砷形态化合物的方法,快速、准确、灵敏,可应用于人群尿砷的测定。[Objective]To establish an High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry(HPLCICP-MS)method for determination of six arsenic species in human urine,including arseniccholine(AsC),arsenobetaine(AsB),arsenite(As^(3+)),dimethylarsinic acid(DMA5+),monomethylarsonic acid(MMA5+),and arsenate(As^(5+)).[Methods]The pH value of mobile phase and the content of anhydrous ethanol were optimized.Ammonium carbonate(50 mmol·L^(-1),containing 2%anhydrous ethanol,pH-8.5)mobile phase was selected.Cl−interference was eliminated by He mode.The arsenic species in 10-fold diluted human urine samples were separated by an Hamilton PRP X-100 anionic column.A method for the determination of six arsenic species was established.[Results]Six arsenic species could be separated in 13 minutes.The linear correlation coefficients were above 0.999.The limits of detection were 0.10-0.20μg·L^(-1),and the limits of quantification were 0.30-0.50μg·L^(-1).Precision experiments showed that RSD ranged from 5.96%to 9.07%when adding concentration 0.20μg·L^(-1);from 2.48%to 6.38%when adding concentration 2.00μg·L^(-1);and from 1.41%to 2.57%when adding concentration 5.00μg·L^(-1).Accuracy test showed that the recoveries were 80%-125%.[Conclusion]The established HPLC-ICP-MS method for determination of six arsenic species in human urine is rapid,accurate and sensitive.It can be applied to the determination of arsenic species in human urine.

关 键 词：高效液相色谱 电感耦合等离子体质谱 砷形态化合物 人 尿 

分 类 号：R446[医药卫生—诊断学]