食品科学 ›› 2011, Vol. 32 ›› Issue (18): 202-204.doi: 10.7506/spkx1002-6630-201118043

• 分析检测 • 上一篇    下一篇

高效液相色谱-电感耦合等离子体质谱同时分析鸡肉中洛克沙生、阿散酸和硝苯胂酸

杨丽君,刘玉敏,崔凤杰,郭 伟*,徐成钢,李兆杰   

  1. 威海出入境检验检疫局检验检疫技术中心
  • 出版日期:2011-09-25 发布日期:2011-09-24
  • 基金资助:
    国家质量监督检验检疫总局科研计划项目(2010Ik148)

Simultaneous Determination of Roxarsone, Arsanilic and Nitarsone in Chicken by High Performance Liquid Chromatography/Inductively Coupled Plasma Mass Spectrometry

YANG Li-jun,LIU Yu-min,CUI Feng-jie,GUO Wei*,XU Cheng-gang,LI Zhao-jie   

  1. (Inspection and Quarantine Center, Weihai Entry-Exit Inspection and Quarantine Bureau, Weihai 264205, China)
  • Online:2011-09-25 Published:2011-09-24

摘要: 建立一种同时测定鸡肉中洛克沙生、阿散酸和硝苯胂酸等3种有机砷类制剂的高效液相色谱-电感耦合等离子体质谱(high performance liquid chromatography tandem inductively coupled plasma mass spectrometry,HPLC-ICP-MS)分析方法。样品经甲醇溶液提取,采用Phenomenex Luna C18色谱柱,体积分数0.05%的三氟乙酸溶液-甲醇作为流动相进行洗脱,经高效液相色谱分离,电感耦合等离子体质谱进行定性和定量分析。结果表明:1~50μg/kg范围内各砷制剂线性良好,相关系数r2均在0.99以上;在1、2、10μg/kg三个加标水平下进行方法验证,平均回收率为85.4%~103.1%,相对标准偏差为3.3%~7.2%;3种有机砷类制剂的定量限均为1μg/kg。方法重现性好、灵敏度高、前处理简单,各项指标均满足国内外法规要求,适用于鸡肉中有机砷类制剂残留的分析检测。

关键词: 高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS), 洛克沙生, 阿散酸, 硝苯胂酸, 鸡肉, 鸡肝

Abstract: An analytical method was developed to simultaneously determine roxarsone, arsanilic and nitarsone in chicken by high performance liquid chromatography/inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Samples were extracted with methanol/water solution. The chromatographic separation was performed on a Phenomenex Luna C18 using methanol and water (containing 0.05% trifluoroacetic acid) as the mobile phase. Identification and quantification were achieved by using ICP-MS. Good linearity was observed in the range of 1 to 50 μg/kg with correlation coefficients above 0.99. The method was validated at the spike levels of 1, 2, 10 μg/kg. The validation results indicated that the average recoveries of arsenicum praeparatum ranged from 85.4% to 103.1% with a relative standard deviation of 3.3%-7.2%. The quantification limits of 3 arsenicum praeparatum were 1μg/kg. The method had good reproducibility, high sensitivity and simple pre-treatment. Its performance could meet both domestic and international legislation requirements. This method is applicable for simultaneous determination of arsenicum praeparatum in chicken.

Key words: high performance liquid chromatography/inductively coupled plasma mass spectrometry (HPLC-ICP-MS), arsanilic, nitarsone, roxarsone, chicken, chicken liver

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