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高效液相色谱-电感耦合等离子体串联质谱法同时测定土壤中的阿散酸、洛克沙胂及其降解产物
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安娅丽,赵艳萍,刘宁,班睿 1.贵州民族大学生态环境工程学院 2.广东省测试分析研究所广东省化学危害应急检测技术重点实验室广东省水环境污染在线监测工程技术研究中心 
基金项目:广东省科学院发展专项资金项目(2019GDASYL-0103023);贵州省科技计划项目(黔科合支撑[2017]2861,黔科合基础[2018]1081)
中文摘要:建立了高效液相色谱-电感耦合等离子体串联质谱(HPLC-ICP-MS/MS)同时测定土壤中阿散酸(p ASA)、洛克沙胂(ROX)及其降解产物无机砷(i-As)(亚砷酸(As(Ⅲ))和砷酸(As(Ⅴ)))、一甲基砷(MMA)和 二甲基砷(DMA)等5种砷形态的分析方法。以0.1 mol/L NaH2PO4-0.1 mol/L H3PO4(体积比9∶1)为提取剂,液固比为50 mL/g,样品经微波辅助提取(80 ℃,30 min)后,采用Hamilton PRP-X100 阴离子交换柱(250 mm×41 mm,10 μm),以60 mmol/L(NH4)2HPO4-5%甲醇(pH 6.0)和水为流动相进行梯度洗脱,在15 min内实现了5种砷形态的良好分离。在优化条件下,各砷形态在0~500 μg/L范围内线性良好(r2≥0.999 1),检出限为0.043~0.080 μg/kg(以As计),相对标准偏差为1.7%~3.8%。将该方法用于分析3种土壤样品,各砷形态的加标回收率为71.6%~106%。该方法简单、快速、准确、可靠,适用于土壤中阿散酸、洛克沙胂和常规砷形态的检测。
中文关键词:高效液相色谱  电感耦合等离子体串联质谱  微波辅助萃取  砷形态分析  土壤
 
Simultaneous Determination of p-Arsanilic Acid,Roxarsone and Their Degradation Products in Soils by HPLC-ICP-MS/MS
Abstract:A high performance liquid chromatography-inductively coupled plasma-tandem mass spectrometry(HPLC-ICP-MS/MS) was developed for the simultaneous determination of six arsenic species,i.ep-arsanilic acid(p-ASA),roxarsone(ROX) and their degradation products arsenite(As(Ⅲ)) and arsenate(As(Ⅴ))(inorganic arsenic),monomethylated arsenic(MMA) and dimethylated arsenic(DMA) in soils.The soil samples were extracted with 0.1 mol/L NaH2PO4-01 mol/L H3PO4(9∶1,by volume) as extraction solvent at a liquid to solid ratio of 50 mL/g,by microwave assisted extraction at 80 ℃ for 30 min.Five arsenic species in the extracts were well separated within 15 min on a Hamilton PRP-X100 anion exchange column(250 mm×4.1 mm,10 μm) using 60 mmol/L(NH4)2HPO4 containing 5% methanol(pH 6.0) and water as mobile phases by gradient elution.Under the optimized conditions,there were good linear relationships for the analytes in the concentration range of 0-500 μg/L with their correlation coefficients(r2) not less than 0.999 1.The limits of detection were 0.043-0080 μg/kg for the analytes,and the relative standard deviations ranged from 1.7% to 3.8%.The method was applied in the analysis of three soil samples,and recoveries for the analytes were in the ranges of 71.6%-106%.The developed method is simple,rapid,accurate and reliable,and is suitable for the determination of arsenic species in soils.
Key Words:high performance liquid chromatography  inductively coupled plasma-tandem mass spectrometry  microwave assisted extraction  arsenic species analysis  soil
引用本文:安娅丽,赵艳萍,刘宁,班睿.高效液相色谱-电感耦合等离子体串联质谱法同时测定土壤中的阿散酸、洛克沙胂及其降解产物[J].分析测试学报,2019,38(11):1353-1357.
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