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机构地区:[1]威海出入境检验检疫局检验检疫技术中心,山东威海264205
出 处:《色谱》2011年第5期394-398,共5页Chinese Journal of Chromatography
基 金:国家质检总局科研计划项目(2010IK148)
摘 要:建立了一种同时测定阿散酸、亚砷酸根、砷酸根、砷胆碱、砷甜菜碱、一甲基砷和二甲基砷等7种砷形态的高效液相色谱-电感耦合等离子体质谱分析方法。样品采用人工胃液作为提取液进行超声处理,再以碳酸铵溶液和水作为流动相,采用阴离子分析柱将样品提取液进行分离,最后进入电感耦合等离子体质谱测定。各砷形态在1~50μg/kg范围内线性关系良好,相关系数r2均在0.999以上;在1、2、10μg/kg 3个添加水平进行了方法学验证,平均回收率为84.3%~106.6%,相对标准偏差为1.4%~4.2%;7种砷形态的定量限均为1μg/kg。方法重现性好、灵敏度高、前处理简单,适用于鸡肉和鸡肝中主要有机砷和无机砷残留的分析检测。A method for the simultaneous determination of 7 arsenic species was developed with high performance liquid chromatography and inductively coupled plasma mass spectrometry(HPLC-ICP-MS).The sample was extracted with artificial gastric juice.The HPLC separation was performed on an anion analytical column utilizing a gradient elution program of ammonium carbonate and water as the mobile phase.Identification and quantification were achieved by ICP-MS.Good linearities of 7 arsenic species were observed in the range from 1 μg/kg to 50 μg/kg with the correlation coefficients greater than 0.999.The average recoveries of 7 arsenic species spiked at the three levels of 1,2 and 10 μg/kg ranged from 84.3% to 106.6% with the relative standard deviations of 1.4%-4.2%.The quantification limits of 7 arsenic species were 1 μg/kg.The method was proved to be good reproducibility,high sensitivity and simple pre-processing.This method is suitable for the simultaneous determination of 7 arsenic species in chicken muscle and chicken liver.
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