Xinjiang Agricultural Sciences

Xinjiang Agricultural Sciences ›› 2019, Vol. 56 ›› Issue (7): 1325-1332.DOI: 10.6048/j.issn.1001-4330.2019.07.016

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Determination of Malachite Green and Leuco Malachite Green in Cold Water Fish in Xinjiang by UPLC-MS/MS MethodUPLC-MS/MS

LI Xiao-yan1, WU Yun2, WANG Li-ye2, SU Min1, SHEN Hui-hui1, Bakhetgul Manatbay1   

  1. 1. Inspection and Quarantine Technology Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China;
    2. College of Animal Sciences, Xinjiang Agricultural University, Urumqi 830052, China
  • Received:2019-05-08 Online:2019-07-20 Published:2019-09-05
  • Correspondence author: WU Yun (1965-), female, Urumqi, Professor, master, research direction: the Food Technology and Safety, (E-mail) wuyunster@sina.com
  • Supported by:
    Supported by S & T Research Project of General Administration of Quality Supervision, Inspection and Quarantie of the People's Republic of China (2007IK174)

UPLC-MS/MS法测定新疆冷水鱼中孔雀石绿与隐色孔雀石绿

李晓岩1, 武运2, 王犁烨2, 苏敏1, 沈慧慧1, 巴哈提古丽·马那提拜1   

  1. 1.新疆出入境检验检疫局技术中心,乌鲁木齐 830063;
    2. 新疆农业大学,乌鲁木齐 830052
  • 通讯作者: 武运(1965-),女,新疆乌鲁木齐人,教授,硕士,研究方向为食品工艺与安全,(E-mail)wuyunster@sina.com
  • 作者简介:李晓岩(1981-),男,新疆乌鲁木齐人,工程师,硕士,研究方向为食品检验,(E-mail)28277391@qq.com
  • 基金资助:
    国家质量监督检验检疫总局科研项目(2007IK174)

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Abstract: 【Objective】 This project aims to establish a more convenient ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of malachite green (MG) and leuco malachite green (LMG) residues in cold water fish in Xinjiang. 【Method】 The sample was extracted with 1% glacial acetic acid-acetonitrile solution, purified by amino and SCX (strong cation exchange) solid phase cartridges, separated by C18 column, and multi-reaction monitoring scanning mode (MRM) of electrospray ionization tandem mass spectrometry, detected and quantified by internal standard method. 【Result】 MG and LMG had a good linear relationship in the linear range of 5.0-100.0 μg/L, and the correlation coefficients were 0.999,7 (MG) and 0.999,2 (LMG), respectively. The lower limit of determination (LOQ) was 2.0 μg/kg. The test was carried out by adding blank sample as the matrix. The recovery rate of MG was 88%-105%, the recovery rate of LMG was 85%-110%, and the relative standard deviation (n=6) was 2.2%-15.3%. 【Conclusion】 The method has the advantages of simple pretreatment, high recovery rate and good stability, whcih is suitable for routine testing of mg and lmg residues in cold water fish in Xinjiang.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS); Xinjiang cold water fish; malachite green; leuco malachite green

摘要： 【目的】建立新疆冷水鱼中孔雀石绿(MG)和隐色孔雀石绿(LMG)残留量的超高效液相色谱－串联质谱(UPLC-MS/MS)更为简便、高效的检测方法。【方法】样品经1%冰乙酸-乙腈溶液提取,氨基及SCX(强阳离子交换)固相小柱净化,C18 色谱柱分离,电喷雾串联四极杆质谱的多反应监测扫描模式(MRM)进行检测,并采用内标法定量。【结果】MG和LMG在5.0～100.0 μg/L线性范围内具有良好的线性关系,相关系数分别为:0.999 7(MG)和0.999 2 (LMG)。测定低限(LOQ)为2.0 μg/kg。以空白样品为基体做加标回收,测得MG的回收率在88%～105%,LMG的回收率在85%～110%,相对标准偏差(n=6)均为2.2%～15.3%。【结论】该方法样品前处理简便,回收率高,稳定性好。适用于新疆冷水鱼中MG和LMG残留量的日常检测。

关键词: 超高效液相色谱－串联质谱, 新疆冷水鱼, 孔雀石绿, 隐色孔雀石绿

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