色谱

色谱 ›› 2014, Vol. 32 ›› Issue (7): 717-722.DOI: 10.3724/SP.J.1123.2014.03015

• 研究论文 • 上一篇    下一篇

液相色谱-电感耦合等离子体质谱法测定稻米中的5种砷形态

巩佳第, 曹晓林, 曹赵云, 卞英芳, 于莎莎, 陈铭学   

  1. 中国水稻研究所 农业部稻米及制品质量监督检验测试中心, 浙江 杭州 310006
  • 收稿日期:2014-03-12 修回日期:2014-05-05 出版日期:2014-07-08 发布日期:2014-06-25
  • 通讯作者: 陈铭学，E-mail：cmingxue@163.com.
  • 基金资助:

    浙江省重点科技创新团队项目（2012R10028-05）.

Determination of five arsenic species in rice by liquid chromatography-inductively coupled plasma-mass spectrometry

GONG Jiadi, CAO Xiaolin, CAO Zhaoyun, BIAN Yingfang, YU Shasha, CHEN Mingxue   

  1. China National Rice Research Institute, Rice Product Quality Inspection and Supervision Center of Ministry of Agriculture, Hangzhou 310006, China
  • Received:2014-03-12 Revised:2014-05-05 Online:2014-07-08 Published:2014-06-25

PDF

271

被引次数

14

摘要：

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0.05~200 μg/L，As（Ⅲ）和MMA为0.10~400 μg/L，As（V）为0.15~600 μg/L，方法检出限为0.15~0.45 μg/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。

关键词: 稻米, 电感耦合等离子体质谱, 砷形态, 石墨消解, 硝酸, 液相色谱

Abstract:

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-assistant 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 standard 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.

Key words: arsenic species, graphite digestion, inductively coupled plasma-mass spectrometry (ICP-MS), liquid chromatography (LC), nitric acid, rice

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