液相色谱-原子荧光法测定大米中4种砷形态
目的 建立以0.3 mol/L硝酸为提取剂提取大米中4种砷形态(亚砷酸根As III、砷酸根As V、一甲基砷MMA和二甲基砷DMA)的液相色谱-原子荧光(liquid chromatography-atomic fluorescence spectrometry, LC-AFS)分析方法。方法 在60 ℃条件下, 超声40 min提取大米样品, 上清液供 LC-AFS 测。比较2种提取方法对稻米中4种砷形态的提取效率, 并对提取温度和提取时间等条件进行优化。结果 4种砷形态化合物的检出限为0.002~0.01 μg/mL, 加标回收率为89.03%~100.70%, RSD不大于4.36%(n=5)。结论 此方法可以在1 h时内完全分离大米样品中的四种砷形态, 操作简单、灵敏, 适用于大米中重金属砷的风险评估。
Objective Using 0.3 mol/L nitric acid as the extractant, to establish a method for the simultaneous determination of arsenious acid (As III), arsenic acid (As V), dimethylarsinic acid (DMA) and monomethylarsinic acid (MMA) in rice by liquid chromatography-atomic fluorescence spectrometry (LC-AFS). Methods After ultrasonic extraction 40 min at 60 ℃, the sample was detected by LC-AFS. The extraction efficiency of two kinds of extracted methods was compared. The concentration of nitric acid, extraction temperature and extraction time were optimized. Results The detection limits of 4 kinds of main arsenic species ( As III, As V, DMA, MMA ) in rice were 0.002~0.01 μg/mL, the recoveries were in the range of 89.03%~100.70%, and the relative standard deviations (RSDs) were less than 4.36%(n=5). Conclusion This method can completely separate the 4 kinds of arsenic species in rice samples within 1 h, which is simple, accurate for the risk assessment of heavy metal arsenic in rice.
标题：液相色谱-原子荧光法测定大米中4种砷形态
英文标题：Determination of 4 kinds of arsenic species in rice by liquid chromatography- atomic fluorescence spectrometry
作者：
魏茂琼 农业部农产品质量安全风险评估实验室(昆明),云南省农业科学院质量标准与检测技术研究所
刘宏程 农业部农产品质量安全风险评估实验室(昆明),云南省农业科学院质量标准与检测技术研究所
严红梅 云南省农业科学院质量标准与检测技术研究所
和立忠 云南省农业科学院质量标准与检测技术研究所
王丽 云南省农业科学院质量标准与检测技术研究所
林昕 农业部农产品质量安全风险评估实验室(昆明),云南省农业科学院质量标准与检测技术研究所
兰珊珊 农业部农产品质量安全风险评估实验室昆明
中文关键词:大米,砷形态,超声提取,液相色谱-原子荧光法,硝酸,
英文关键词:rice,arsenic species,ultrasonic extraction,liquid chromatography-atomic fluorescence spectrometry,nitric acid,
发表日期：2016-08-04
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