高效液相色谱-电感耦合等离子体质谱法测定大米中无机砷

目的建立高效液相色谱-电感耦合等离子体质谱法测定大米中无机砷的分析方法。方法采用两种前处理方法对大米中的无机砷进行提取,经高效液相色谱分离后,利用电感耦合等离子体质谱进行测定。同时对大米样品进行微波消解后测定其中的总砷,通过无机砷及有机砷的总和计算两种前处理方法的回收率,从而对前处理方法进行比较。对磷酸二氢铵、碳酸铵以及磷酸氢二铵等缓冲盐进行选择,并对p H值进行优化,确定最优的流动相条件。结果以12.5 mmol/L磷酸氢二铵作为流动相,调节流动相p H为8.5,流速为1 m L/min,可以将5种无机砷形态完全分离。对两种前处理方法进行比较,发现两种前处理方法的提取效率均大于87.5%,其...

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Published in食品安全质量检测学报 Vol. 8; no. 2; pp. 569 - 573
Main Author 史潜玉 刘立 倪志尧 柯润辉 赵欣 尹建军 宋全厚
Format Journal Article
LanguageChinese
Published 国家食品质量监督检验中心,北京 100015%聚光科技(杭州)股份有限公司,杭州,310052 2017
中国食品发酵工业研究院,北京 100015
Subjects
形态分析
无机砷
电感耦合等离子体质谱法
高效液相色谱法
电感耦合等离子体质谱法
high performance liquid chromatography
无机砷
形态分析
高效液相色谱法
inductively coupled plasma mass spectrometry
inorganic arsenic
morphological analysis
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ISSN2095-0381

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Summary:目的建立高效液相色谱-电感耦合等离子体质谱法测定大米中无机砷的分析方法。方法采用两种前处理方法对大米中的无机砷进行提取,经高效液相色谱分离后,利用电感耦合等离子体质谱进行测定。同时对大米样品进行微波消解后测定其中的总砷,通过无机砷及有机砷的总和计算两种前处理方法的回收率,从而对前处理方法进行比较。对磷酸二氢铵、碳酸铵以及磷酸氢二铵等缓冲盐进行选择,并对p H值进行优化,确定最优的流动相条件。结果以12.5 mmol/L磷酸氢二铵作为流动相,调节流动相p H为8.5,流速为1 m L/min,可以将5种无机砷形态完全分离。对两种前处理方法进行比较,发现两种前处理方法的提取效率均大于87.5%,其中酸-热辅助提取法的提取效率相对更高。结论该方法准确、简单,适合大米中无机砷的测定。
Bibliography:Objective To establish a method for determination of inorganic arsenic in rice by high performance liquid chromatography-inductively coupled plasma mass spectrometry（HPLC-ICP-MS）. Methods Inorganic arsenic in rice was extracted by 2 kinds of pretreatment methods. After separated by HPLC, the samples were determined by ICP-MS. At the same time, the total arsenic of rice samples was determined after microwave digestion. The recoveries of 2 pretreatment methods were calculated by the sum of inorganic arsenic and organic arsenic, and the pretreatment methods were compared. The buffer salts such as ammonium dihydrogen phosphate, ammonium carbonate and diammonium hydrogen phosphate were selected and the p H value was optimized to confirm the optimum mobile phase conditions. Results In this method, 12.5 mmol/L diammonium hydrogen phosphate was used as the mobile phase, the mobile phase was adjusted to pH 8.5 and the flow rate was 1 mL/min. Under such conditions, 5 kinds of inorganic arsenic species could be separate
ISSN:2095-0381