色谱 ›› 2011, Vol. 29 ›› Issue (05): 394-398.DOI: 10.3724/SP.J.1123.2011.00394

• 研究论文 • 上一篇    下一篇

高效液相色谱-电感耦合等离子体质谱联用同时测定鸡肉与鸡肝中的7种砷形态

杨丽君, 胡巧茹, 郭伟*, 刘玉敏, 宋晓华, 张鹏程   

  1. 威海出入境检验检疫局检验检疫技术中心, 山东 威海 264205
  • 收稿日期:2010-12-21 修回日期:2011-02-11 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 郭伟,硕士,主要从事食品检测
  • 基金资助:
    国家质检总局科研计划项目(2010IK148).

Simultaneous determination of 7 arsenic species in chicken muscle and chicken liver with high performance liquid chromatography-inductively coupled plasma mass spectrometry

YANG Lijun, HU Qiaoru, GUO Wei*, LIU Yumin, SONG Xiaohua, ZHANG Pengcheng   

  1. Inspection and Quarantine Technique Center, Weihai Entry-Exit Inspection and Quarantine Bureau, Weihai 264205, China
  • Received:2010-12-21 Revised:2011-02-11 Online:2011-05-28 Published:2011-05-28

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1~50 μg/kg范围内线性关系良好,相关系数r2均在0.999以上;在1、2、10 μg/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1 μg/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。

关键词: 电感耦合等离子体质谱, 高效液相色谱, 鸡肝, 鸡肉, 无机砷, 有机砷

Abstract: 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.

Key words: chicken liver, chicken muscle, organic arsenic, high performance liquid chromatography (HPLC), inductively coupled plasma mass spectrometry (ICP-MS), inorganic arsenic