Andersen Wendy C, Turnipseed Sherri B, Roybal José E
Animal Drugs Research Center, Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, Colorado 80225-0087, USA.
J Agric Food Chem. 2006 Jun 28;54(13):4517-23. doi: 10.1021/jf0532258.
Liquid chromatographic methods are presented for the quantitative and confirmatory determination of malachite green (MG) and leucomalachite green (LMG) for channel catfish, rainbow trout, tilapia, basa, Atlantic salmon, and tiger shrimp. Residues were extracted from tissues with ammonium acetate buffer and acetonitrile and isolated by partitioning into dichloromethane. LMG was quantitatively oxidized to the chromic MG with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone. Extracts were analyzed for total MG by liquid chromatography with both visible detection (LC-VIS) at 618 nm for routine screening and ion trap mass spectrometry (LC-MSn) with no discharge-atmospheric pressure chemical ionization for residue confirmation. The method was validated in each species fortified with LMG at 1, 2, 4, and 10 ng/g (ppb), and average recoveries ranged from 85.9 to 93.9%. Quantitative data were consistent for the two detection methods, with measured method detection limits of 1.0 ng/g for LC-VIS and 0.25 ng/g for LC-MSn. Incurred tissues from catfish, trout, tilapia, and salmon that had been treated with MG were also extracted and analyzed as part of this study.
本文介绍了用于定量和确证测定斑点叉尾鮰、虹鳟、罗非鱼、巴沙鱼、大西洋鲑和虎虾中孔雀石绿（MG）和无色孔雀石绿（LMG）的液相色谱方法。用醋酸铵缓冲液和乙腈从组织中提取残留物，并通过分配到二氯甲烷中进行分离。用2,3 - 二氯 - 5,6 - 二氰基 - 1,4 - 苯醌将LMG定量氧化为有色的MG。提取物通过液相色谱进行分析，常规筛查采用618 nm可见光检测（LC - VIS），残留物确证采用无放电大气压化学电离的离子阱质谱（LC - MSn）。该方法在每种添加了1、2、4和10 ng/g（ppb）LMG的物种中进行了验证，平均回收率在85.9%至93.9%之间。两种检测方法的定量数据一致，LC - VIS的实测方法检测限为1.0 ng/g，LC - MSn为0.25 ng/g。作为本研究的一部分，还对用MG处理过的斑点叉尾鮰、鳟鱼、罗非鱼和鲑鱼的实际组织进行了提取和分析。
