王丽敏, 杜雪莉, 赵艳, 刘耀敏. 超高效液相色谱－串联质谱快速测定水产品中孔雀石绿、结晶紫及其代谢物残留[J]. 南方水产科学, 2010, 6(4): 32-36. DOI: 10.3969/j.issn.1673-2227.2010.04.006
引用本文: 王丽敏, 杜雪莉, 赵艳, 刘耀敏. 超高效液相色谱－串联质谱快速测定水产品中孔雀石绿、结晶紫及其代谢物残留[J]. 南方水产科学, 2010, 6(4): 32-36. DOI: 10.3969/j.issn.1673-2227.2010.04.006
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 WANG Limin, DU Xueli, ZHAO Yan, LIU Yaomin. Rapid residue determination of malachite green, crystal violet and their metabolites in aquatic products by UPLC-MS/MS[J]. South China Fisheries Science, 2010, 6(4): 32-36. DOI: 10.3969/j.issn.1673-2227.2010.04.006
Citation:  WANG Limin, DU Xueli, ZHAO Yan, LIU Yaomin. Rapid residue determination of malachite green, crystal violet and their metabolites in aquatic products by UPLC-MS/MS[J]. South China Fisheries Science, 2010, 6(4): 32-36. DOI: 10.3969/j.issn.1673-2227.2010.04.006
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超高效液相色谱－串联质谱快速测定水产品中孔雀石绿、结晶紫及其代谢物残留

Rapid residue determination of malachite green, crystal violet and their metabolites in aquatic products by UPLC-MS/MS

    摘要
  • 摘要: 建立了超高效液相色谱-串联质谱（UPLC-MS/MS）测定水产品中孔雀石绿（MG）、结晶紫（CV）及其代谢物隐色孔雀石绿（LMG）和隐色结晶紫（LCV）残留量的快速、准确检测方法。该法在SN/T 1768-2006快速检测方法的基础上，采用空白样品添加不同质量浓度标准溶液的方式绘制校准曲线，并以氘代孔雀石绿（D5-MG）和氘代隐色孔雀石绿（D6-LMG）为内标进行检测，从而大大提高了定量的准确性。结果表明，MG、CV、LMG和LCV 4种待测物在0~10.0 ngmL-1范围内线性关系良好（R0.99），方法检出限均为0.1 gkg-1。在加标量为0.5和1.0 gkg-1水平下4种待测物平均回收率在92.1%~111.0%之间，测定结果的相对标准偏差为2.2%~9.5%。此外，该法在FAPAS国际能力验证中得以证实，改进后的方法快速且准确，能满足水产品出口检测要求。

     

    Abstract: We developed a rapid and accurate method by UPLC-MS/MS to determine the residue of malachite green (MG) ,crystal violet (CV) and their metabolites (LMG and LCV) in aquatic products. Based on the rapid method of SN/T 1768-2006, standard curves were made by adding standard solutions of different concentrations to the blank samples, and D5-MG and D6-LMG were used as internal standards, which improved the accuracy of determination. The results show that MG, CV, LMG and LCV have a good linear correlation within the range of 0~10.0 ngmL-1 (R0.99), and the detection limits of the method are all 0.1 gkg-1. The average recoveries at fortification of 0.5 and 1.0 gkg-1 range from 92.1% to 111.0% with relative standard deviations (RSD) varyingfrom 2.2% to 9.5%. Furthermore, the rapid and accurate improved method is also proved by FAPAS Proficiency Test to meet the export testing requirements of aquatic products.

     

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