| 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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| 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) |
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| 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×41 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 |
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| Simultaneous Determination of p-Arsanilic Acid,Roxarsone and Their Degradation Products in Soils by HPLC-ICP-MS/MS |
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| 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.ep-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 NaH2PO4-01 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 0.043-0080 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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