双柱在线净化快速测定鱼肉中孔雀石绿、结晶紫及其代谢物
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摘要
建立鱼肉中的孔雀石绿、结晶紫及隐色代谢物的双柱在线净化(阳离子净化柱MCX一维净化,反相C8净化柱二维净化)-高效液相色谱-串联质谱测定方法。采用酸性乙腈提取样品,提取液直接上机分析,双柱在线净化系统净化,高效液相色谱-串联质谱测定。结果表明,鱼肉中孔雀石绿、结晶紫、隐色孔雀石绿、隐色结晶紫空白鱼肉3个不同水平的添加回收率(n=6)为76.8%～109.4%,相对标准偏差为2.0%～14.1%,4种药物定量限为0.5μg/kg。
A double column on-line purification was builded through combining the first purification of MCX column and the second purification of C8 column to determine the residues of malachite green,crystal ciolet and their leuco metabolites in fish by high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with acid acetonitrile. The extract was directly injected into double column on-line purification system. The results showed that the average recoveries of three levels were from 76.8 % to 109.4 %,and the relative standard deviation ranged from 2.0 % to 14.1 %.The detection limits of the four drugs were0.5 μg/kg.
A double column on-line purification was builded through combining the first purification of MCX column and the second purification of C8 column to determine the residues of malachite green,crystal ciolet and their leuco metabolites in fish by high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with acid acetonitrile. The extract was directly injected into double column on-line purification system. The results showed that the average recoveries of three levels were from 76.8 % to 109.4 %,and the relative standard deviation ranged from 2.0 % to 14.1 %.The detection limits of the four drugs were0.5 μg/kg.
引文
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[15]堵燕钰,罗漪涟,吴冬梅,等.在线净化/LC-MS-MS测定淡水鱼中孔雀石绿及隐性孔雀石绿[J].常州大学学报(自然科学版),2015,27(1):71-75
[2]翟毓秀,郭莹莹,耿霞,等.孔雀石绿的代谢机理及生物毒性研究进展[J].中国海洋大学学报,2007,37(1):27-32
[3]刘军,胡华军,张明渊,等.鱼药孔雀石绿的毒性、危害和检测现状[J].浙江农业学报,2006,18(5):337-340
[4]郭德华,叶长淋,朱莹洁.液相色谱法测定鳗鱼中孔雀石绿[J].化学分析计量,2002,11(2):20-21
[5]张彤晴,杨洪生,林海,等.高效液相色谱法测定养殖水体中孔雀石绿和无色孔雀石绿[J].水产学报,2007,31(5):609-703
[6]V alle L,D iaz C,Zanocco A L,et a1.Determination of the sum of malachitegreen and leucmalachite green in salm on muscle by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry[J].Journal of Chromatography A,2005,1067(1-2):101-105
[7]赵东豪,黎智广,林钦,等.高效液相色谱串联质谱测定沉积物中的孔雀石绿、结晶紫及其隐色代谢物[J].广东农业科学,2011,38(2):17l-173
[8]高华鹏,李永夫,沈维军,等.高效液相色谱-串联质谱联用测定鳗鱼中孔雀石绿、结晶紫及其代谢物残留量[J].理化检验:化学分册,2008,44(2):103-106
[9]周贻兵,吴坤,刘利亚,等.超高效液相色谱-串联质谱法测定鱼中孔雀石绿、结晶紫及其代谢物残留量[J].质谱学报,2013,34(5):294-299
[10]冯富,孙文通,李波,等.水产品中残留孔雀石绿和无色孔雀石绿液质联用分析方法研究[J].食品科学,2009,30(4):193-196
[11]朱宽正,王鹏,林雁飞,等.液相色谱-串联质谱法同时测定水产品中孔雀石绿、结晶紫以及它们的隐色代谢物残留[J].色谱,2007,25(1):66-69
[12]Holtzapple C K,Buckley S A,Stanker L H.Determination of fluoroquinolones in serum using an on-line clean-up column coupled to high-performance immunoaffinity-reversed-phase liquid chromatography[J].Journal of chromatogr B Biomed Sci Appl,2001,754(1):1-9
[13]李丹妮,严凤,吴剑平,等.在线净化液相色谱-串联质谱法测定畜禽粪便中7种β-受体激动剂[J].分析化学,2014,42(12):1797-1803
[14]曹亚青,宋歌,王曼曼,等.Turbo FIow在线净化/液相色谱-串联质谱法快速测定动物源性食品中聚醚类抗生素的研究[J].分析测试学报,2016,35(10):1273-1277
[15]堵燕钰,罗漪涟,吴冬梅,等.在线净化/LC-MS-MS测定淡水鱼中孔雀石绿及隐性孔雀石绿[J].常州大学学报(自然科学版),2015,27(1):71-75