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首页> 外文期刊>Food additives & contaminants >Validation of an LC-MS/MS method for malachite green (MG), leucomalachite green (LMG), crystal violet (CV) and leucocrystal violet (LCV) residues in fish and shrimp
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Validation of an LC-MS/MS method for malachite green (MG), leucomalachite green (LMG), crystal violet (CV) and leucocrystal violet (LCV) residues in fish and shrimp

机译：LC-MS / MS方法对鱼虾中的孔雀石绿（MG），白孔雀绿（LMG），结晶紫（CV）和无色结晶紫（LCV）残留的验证

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摘要

A quantitative liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous analyses of malachite green (MG), crystal violet (CV) and its major metabolites, leucomalachite green (LMG) and leucocrystal violet (LCV) residues in fish and shrimp samples has been validated. Fish and shrimp samples were extracted with citrate buffer/acetonitrile, and the extracts were purified on strong cation-exchange (SCX) solid-phase extraction (SPE) cartridge. After conversion of LMG into MG using a post column oxidation reactor containing lead (IV) oxide (PbO_2), the effluents were analysed. Residues were analysed using positive-ion electrospray ionisation (ESI). Identification and quantification of analytes were based on the ion transitions monitored by multiple reaction monitoring (MRM). Validation of the method was carried out in accordance with the Decision 2002/657/EC, which establishes criteria and procedures for the validation of methods. The following parameters were determined: decision limit (CCα), detection capability (CCβ), linearity, accuracy, precision, selectivity, specificity and matrix effect. The decision limits (CCα) for MG, LMG, CV and LCV were 0.164, 0.161, 0.248 and 0.860μg kg~(-1). The respective detection capabilities (CQβ) were 0.222, 0.218, 0.355 and 1.162μg kg~(-1). Typical recoveries (intermediate precision) in shrimp, for MG, CV, LMG and LCV for 2.0μg kg~(-1) level fortified samples using the optimised procedure were in the range 69%, 97%, 80.3% and 71.8%, respectively. The findings demonstrate the suitability of the method to detect simultaneously MG, CV and its metabolite (LMG and LCV) in fish and shrimp.
机译：定量液相色谱-串联质谱（LC-MS / MS）方法用于同时分析孔雀石绿（MG），结晶紫（CV）及其主要代谢产物，白孔雀绿（LMG）和无色结晶紫（LCV）残留鱼和虾样品已经过验证。鱼和虾样品用柠檬酸盐缓冲液/乙腈萃取，萃取物在强阳离子交换（SCX）固相萃取（SPE）柱上纯化。使用含有氧化铅（IV）（PbO_2）的柱后氧化反应器将LMG转化为MG后，对流出物进行了分析。使用阳离子电喷雾电离（ESI）分析残留物。分析物的鉴定和定量是基于通过多反应监测（MRM）监测的离子跃迁。根据第2002/657 / EC号决定对方法进行了验证，该决定建立了方法验证的标准和程序。确定了以下参数：决策极限（CCα），检测能力（CCβ），线性，准确性，精确度，选择性，特异性和基质效应。 MG，LMG，CV和LCV的判定极限（CCα）为0.164、0.161、0.248和0.860μgkg〜（-1）。各自的检测能力（CQβ）分别为0.222、0.218、0.355和1.162μgkg〜（-1）。采用优化程序，对虾中MG，CV，LMG和LCV的2.0μgkg〜（-1）水平强化样品的典型回收率（中等精度）分别在69％，97％，80.3％和71.8％范围内。 。这些发现表明该方法适用于同时检测鱼虾中的MG，CV及其代谢物（LMG和LCV）。

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  • 来源
    《Food additives & contaminants》 |2012年第4期|p.602-608|共7页
  • 作者

    Jociani Ascari; Sergio Dracz; Flavio A. Santos; J.A. Lima; Maria Helena G. Diniz; Eugenia A. Vargas;

  • 作者单位

    Bolsista CNPq, Laboratorio Nacional Agropecuario (LANAGRO), Pedro Leopoldo, Brazil;

    Laboratorio de Residuos de Medicamento Veterindrios, Laboratorio Nacional Agropecudrio (LANAGRO), Pedro Leopoldo, Brazil;

    Laboratorio de Residuos de Medicamento Veterindrios, Laboratorio Nacional Agropecudrio (LANAGRO), Pedro Leopoldo, Brazil;

    Laboratorio de Residuos de Medicamento Veterindrios, Laboratorio Nacional Agropecudrio (LANAGRO), Pedro Leopoldo, Brazil;

    Laboratorio de Residuos de Medicamento Veterindrios, Laboratorio Nacional Agropecudrio (LANAGRO), Pedro Leopoldo, Brazil;

    Laboratorio de Residuos de Medicamento Veterindrios, Laboratorio Nacional Agropecudrio (LANAGRO), Pedro Leopoldo, Brazil;

  • 收录信息 美国《科学引文索引》(SCI);美国《生物学医学文摘》(MEDLINE);美国《化学文摘》(CA);
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

    shrimp; fish; malachite green; leucomalachite green; dyes; analysis; method validation;

    机译：虾;鱼;孔雀石绿;白孔雀石绿;染料;分析;方法验证;

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