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• 分析检测 •    下一篇

超高效液相色谱串联质谱法检测鱼中孔雀石绿、结晶紫及其代谢物

张艺蓓1,岳田利2,乔海鸥3,贾如1,蒋旭鹏1,李璐1   

  1. 1. 西北农林科技大学
    2. 陕西杨凌西北农林科技大学食品科学与工程学院
    3. 陕西省疾病预防控制中心
  • 收稿日期:2013-09-24 修回日期:2014-03-28 出版日期:2014-05-25 发布日期:2014-05-29
  • 通讯作者: 岳田利 E-mail:yuetl@nwsuaf.edu.cn
  • 基金资助:
    2013年西北农林科技大学大学生创新训练计划项目(校级重点)

Determination of Malachite Green, Crystal Violet and Their Metabolites Contents in Fishes by UPLC-MS/MS

Yi-Bei ZHANG Hai-Ou QIAO2,Ru Jia 2, 2   

  • Received:2013-09-24 Revised:2014-03-28 Online:2014-05-25 Published:2014-05-29

摘要: 摘要:目的 采用超高效液相色谱-串联质谱法(Ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定鱼中孔雀石绿(Malachite green, MG)、隐性孔雀石绿(Leuco malachite green, LMG)、结晶紫(Crystal violet, CV)、隐性结晶紫(Leuco crystal violet, LCV)四种物质残留。方法 样品加入内标物d5-MG、d6-LMG、d5-CV、d6-LCV,经乙腈提取、离心、过中性氧化铝柱,氮气吹至近干,乙腈/水(50:50, v/v)定容,上机测定。结果 MG和LMG线性范围为1-50ng/mL,CV和LCV线性范围为1-100ng/mL。四种物质的检出限均为0.05μg/kg,定量限均为0.15μg/kg。在50、100、200ng/mL三个添加水平下,回收率在87.8%-110.8%之间,相对标准偏差均小于4.32%(n=6)。结论 该方法灵敏、准确、可靠,可以同时测定鱼中MG、LMG、CV、LCV残留,为鱼类水产的多残留检测提供了好的检测方法。

关键词: 超高效液相色谱-串联质谱(UPLC-MS/MS), 鱼, 孔雀石绿, 结晶紫, 残留

Abstract: Abstract:Purpose Malachite green (MG), leuco malachite green (LMG), crystal violet (CV)and leuco crystal violet (LCV) residues in fish were determinated simultaneously using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Fish samples added with internal standard d5-MG, d6-LMG, d5-CV, d6-LCV were extracted in acetonitrile at first, and then degreased through neutral alumina column, dried in nitrogen, volumed by solution of acetonitrile distilled water (50:50, V/V) to UPLC-MS/MS analysis. Results The linearity was investigated over a concentration range of 1-50ng/mL for MG and LMG. The linearity was investigated over a concentration range of 1-100ng/mL for CV and LCV. The limit of detection of MG, LMG, CV and LCV are 0.05μg/kg and the limit of quantification of four analyses are 0.15μg/kg. Method recovery is made by addition of 50, 100, 200ng/mL standard solution, respectively. The results show that average recoveries are between 87.8% and 110.8%, and relative standard deviations (RSD, n=6) are lower than 4.32%. Conclusions This method is sensitive, accurate and reliable, which provide reference for multitude residues detection of aquatic fish products.

Key words: Ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), Fish, Malachite green (MG), Crystal violet (CV), Residues

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