QuEChERS/UPLC-MS/MS法测定水产品中孔雀石绿和结晶紫及其代谢物 |
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基金项目:国家质检总局科技项目(2016IK066 );江门市科技项目(20161408 ) |
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中文摘要:建立了水产品中孔雀石绿(MG)和结晶紫(CV)及其代谢物隐色孔雀石绿(LMG)和隐色结晶紫(LCV)残留的QuEChERS/UPLC-MS/MS分析方法。样品采用乙腈提取,改进的QuEChERS(EMR Lipid)分散固相萃取净化,经Agilent Eclipse Plus C18(1.8 μm,3.0 mm×100 mm)色谱柱分离,电喷雾串联四极杆质谱多反应监测正离子方式测定。4种分析物在0.2~10.0 μg/L范围内线性关系良好,相关系数均大于0.997。鱼肉中4种分析物在0.5,1.0,5.0 μg/kg加标浓度水平下,回收率为77.1%~106.6%,相对标准偏差(RSD)为1.3%~4.3%。该方法简单、稳定、可靠,能有效去除样品中的蛋白质、脂肪等大分子杂质,可满足水产品中孔雀石绿、结晶紫以及隐色代谢物残留检测与确证的需要。 |
中文关键词:QuEChERS EMR-Lipid UPLC-MS/MS 孔雀石绿 隐色孔雀石绿 结晶紫 隐色结晶紫 |
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Determination of Malachite Green,Crystal Violet and Their Metabolites Residues in Aquatic Product by QuEChERS Combined with UPLC-MS/MS |
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Abstract:A method for the determination of malachite green(MG),crystal violet(CV) and their metabolites residues leucomalachite green(LMG) and leucocrystal violet(LCV) in aquatic product was developed using QuEChERS combined with UPLC-MS-MS.The sample was extracted with acetonitrile and purified by EMR-Lipid.The target compounds were separated on an Agilent Eclipse Plus C18(1.8 μm,3.0 mm×100 mm) column,and detected by tandem mass spectrometry with electrospray ionization in positive mode.The linear ranges were in the range of 0.2-10.0 μg/L and the correlation coefficients were all above 0.997.The average recoveries of 4 analytes in fish matrix at three spiked concentrations of 0.5,1.0,5.0 μg/kg ranged from 77.1% to 106.6%,with relative standard deviations of 1.3%-4.3%.This method was simple and reliable,and could effectively remove the protein and fat in sample.Therefore,it is suitable for the determination of MG,CV and their leuco metabolites residues in aquatic product. |
Key Words:QuEChERS EMR-Lipid UPLC-MS-MS malachite green(MG) leucomalachite green(LMG) crystal violet(CV) leucocrystal violet(LCV) |
引用本文:宫小明,华萌萌,王洪涛,王炳军,马荣桧.QuEChERS/UPLC-MS/MS法测定水产品中孔雀石绿和结晶紫及其代谢物[J].分析测试学报,2017,36(7):897-901. |
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