建立了稻米中砷酸根[As（V）]、亚砷酸根[As（Ⅲ）]、砷甜菜碱（AsB）、一甲基砷（MMA）和二甲基砷（DMA）的液相色谱-电感耦合等离子体质谱（ LC-ICP-MS）检测方法。以0.3 mol/L硝酸水溶液为提取试剂，样品在石墨消解仪中于95℃消解1.5 h，上清液供 LC-ICP-MS分析。5种砷形态采用 Dionex IonPac AS19阴离子交换柱（250 mm×4 mm）分离，经 ICP-MS检测。比较了4种提取液对稻米中5种砷形态的提取效率，并对提取溶剂的浓度、提取温度和提取时间等条件进行了优化。通过加标回收试验结合测定标准物质考察了方法准确度及精密度，在2个加标水平上各形态的回收率为89.6％~99.5％，RSD（ n=5）不大于3.6％，大米标准物质中各形态之和的测定结果与其标准值吻合，5种砷形态的线性范围 AsB和 DMA为0.05~200μg/L，As（Ⅲ）和MMA为0.10~400μg/L，As （ V）为0.15~600μg/L，方法检出限为0.15~0.45μg/kg。结果表明，本方法简单、灵敏、耐用，可用于稻米中5种砷形态的准确定量和风险评估。
A method was developed for the simultaneous determination of arsenic acid[ As ( V)],arsenious acid[ As(Ⅲ)],arsenobetaine( AsB),monomethylarsonic acid( MMA)and dimethylarsinic acid( DMA)in rice by liquid chromatography-inductively coupled plasma-mass spectrometry( LC-ICP-MS). The extraction reagent was 0. 3 mol/L nitric acid with heat-assis-tant condition for 1. 5 h at 95 ℃. Then,the five arsenic species were separated by an anion exchange column(Dionex IonPac AS19,250 mm×4 mm)and detected by ICP-MS. Four kinds of extracted solutions were compared through the extraction efficiency. The concentration of nitric acid,the temperature and the extraction time were optimized. The recoveries of the five arsenic species spiked in rice at two levels ranged from 89. 6% to 99. 5% with the relative stand-ard deviations(RSDs,n=5)of 0. 6%-3. 6%. The measured values of the arsenic species in standard rice materials were consistent with their standard values. The linear ranges were 0. 05-200 μg/L for AsB and DMA,0. 10-400 μg/L for As(Ⅲ)and MMA,0. 15-600 μg/L for As ( V). The limits of detection for the five arsenic species were 0. 15-0. 45 μg/kg. The results showed that the method is much more precise for the risk assessment of the rice. This method is simple,accurate and durable for the determination of arsenic species in rice.
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