超高效液相色谱-串联质谱法测定水产品中孔雀石绿前处理方法的改进

Improvement of Malachite Green Pretreatment in Aquatic Products by UPLC-MS/MS

  • 摘要: 采用超高效液相色谱-串联质谱法(UPLC-MS/MS)测定水产品中孔雀石绿的残留量,以GB/T 19857-2005检测方法为基础,将前处理步骤进行优化.称取5 g样品,加入质量浓度为100 μg/L的内标标准溶液100 μL,混匀,加入20 mL乙腈、5 g酸性氧化铝,震荡、离心,取4 mL溶液氮气吹干,用流动相定容至1 mL,过0.22 μm滤膜,上机测试.按照标准方法测定标准曲线相关系数r:孔雀石绿为0.999,隐色孔雀石绿为0.999.孔雀石绿的回收率分别为71.7%、95.2%和89.9%,精密度分别为4.47%、4.26%和8.57%.隐色孔雀石绿的回收率分别为93.3%、98.8%和89.7%,精密度分别为8.73%、6.87%和9.71%.试验结果满足相关标准和体系文件的要求.

     

    Abstract: The residue of malachite green in aquatic products was determined by the ultra high performance liquid chromatography-mass spectrometry/mass spectrometry(UPLC-MS/MS), and the pretreatment procedure was optimized based on the GB/T 19857-2005 detection method. 100 μL internal standard solution of mass concentration of 100 μg/L was added to 5 g of sample, and mixed well, then 20 mL of acetonitrile, 5 g of acidic alumina were added, and shocked, centrifuged, then 4 mL of the solution was blown dry by nitrogen to 1 mL, and filtered through a 0.22 μm membrane, and then carried out the test. The correlation coefficient r of the standard curve was determined by the standard method:both malachite green, and cryptochrome malachite were 0.999. The recovery rate of malachite green was 71.7%, 95.2% and 89.9% respectively, and the precision was 4.47%, 4.26% and 8.57% respectively. The recovery rates of cryptochrome malachite green were 93.3%, 98.8% and 89.7% respectively, and the precision was 8.73%, 6.87% and 9.71%, respectively. The test results met the requirements of relevant standards and system documents.

     

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