隐性孔雀石绿残留量-现代科学仪器.PDFVIP

高效液相色谱－串联质谱联用(Finnigan TSQ Quantum)测定 鳗鱼中孔雀石绿、隐性孔雀石绿残留量 1 1 1 1 1 2 丁涛 徐锦忠 吴斌 陈惠兰 沈崇钰 刘飞 1 （江苏出入境检验检疫局食品实验室 南京 210001 ） 2 热电上海科学仪器公司示范实验室 上海 201206 ） （ 摘 要 利用高效液相色谱串联质谱（LC/MS/MS ）方法快速、准确的同时测定鳗鱼中孔雀石绿、隐性孔雀石绿残留 量。鳗鱼样品经乙腈- 乙酸铵缓冲溶液提取，液相色谱分配到二氯甲烷层，MCX 阳离子固相萃取小柱净化，浓缩定容。以甲 醇和甲酸缓冲溶液为流动相，经C18 柱分离后，并用串联质谱在电喷雾（ESI+ ）- 选择反应监测离子（SRM）的模式下，氘代 隐性孔雀石绿为内标，进行质谱定性和定量。该方法无需采用传统PbO2 氧化柱，检测限（LOD ）为0.2μg/Kg ，定量下限为 0.5 μg/Kg ，完全可以达到出口欧盟和日本残留限量要求。 关键词 高效液相色谱－串联质谱；电喷雾串联质谱；孔雀石绿；隐性孔雀石绿；鳗鱼 中图分类号 O657.63 Determination of Residues of Malachite Green and Leuco-malachite Green in Eel by Liquid Chromatography Tandem Mass Spectrometry 1 1 1 1 1 2 Ding Tao , Xu Jinzhong , Wu Bin , Chen Huilan , Shen Chongyu , Liu Fei 1 ( Jiangsu Entry-Exit Inspection and Quarantine Bureau, Animal, Plant and Food Inspection Center- APFIC, National Honey Refer- ence Lab, Nanjing 210001, China)(2Thermo Electron Corporation, Shanghai201206, China) Abstract A quick and accurate LC/MS/MS method is presented to simultaneously detect Malachite green (MG) and Leuco-malachite green (LMG) residues in eel. After extracting by acetonitrile-ammonium acetate buffer solutions and dichloromethane, the extracts were purified by anion exchange cartridge (MCX) for LC/MS/MS analysis. The residues were separated on liquid chromatography with a reverse phase C18 column using methanol and formic acid solution as mobile phase, and detected on a Finnigan TSQ Quantum Ultra model triple quadrupole mass spectrometry operated in selecte