Plakas S M, el Said K R, Stehly G R, Roybal J E
U.S. Food and Drug Administration, Gulf Coast Seafood Laboratory, Dauphin Island, AL 36528, USA.
J AOAC Int. 1995 Nov-Dec;78(6):1388-94.
A liquid chromatographic (LC) method was adapted and optimized for the determination of malachite green and its metabolites in fish plasma and muscle. Residues in plasma were extracted with acetonitrile, the extract was evaporated to dryness, and residues were resolubilized for LC analysis. Residues in muscle were extracted with an acetonitrile-acetate buffer mixture, reextracted with acetonitrile, and partitioned into methylene chloride with final cleanup on alumni and propylsulfonic acid solid-phase extraction columns. Residue levels were determined by using an LC cyano column with a PbO2 postcolumn and visible detection (618 nm). Overall mean recoveries of parent malachite green (MG-C) and its major metabolite, leuco-malachite green (MG-L), from plasma were 93 and 87%,respectively, at fortification levels ranging from 25 to 250 ppb. Overall mean recoveries of MG-C and MG-L from muscle were 85 and 95%, respectively, at fortification levels ranging from 5 to 100 ppb. Relative standard deviations (RSDs) of recoveries at all fortification levels ranged from 3.9 to 7.0% for plasma and from 2.1 to 5.2% for muscle. The method was applied to incurred residues in tissues sampled from catfish after waterborne exposure to [14C]MG-C. Mean recoveries of total radioactive residues in plasma and muscle throughout the extraction and cleanup process were 88 and 87%, respectively, and corresponding RSDs for MG-C and MG-L were in the same range as those for fortified tissues. MG-L was confirmed as the major metabolite of MG-C in catfish.
一种液相色谱（LC）方法被调整并优化，用于测定鱼血浆和肌肉中的孔雀石绿及其代谢物。血浆中的残留物用乙腈提取，提取物蒸发至干，残留物重新溶解用于LC分析。肌肉中的残留物先用乙腈 - 醋酸盐缓冲液混合物提取，再用乙腈重新提取，然后用二氯甲烷分配，最后在铝和丙基磺酸固相萃取柱上进行净化。残留物水平通过使用带有PbO2柱后和可见光检测（618 nm）的LC氰基柱来测定。在25至250 ppb的强化水平下，血浆中母体孔雀石绿（MG-C）及其主要代谢物隐色孔雀石绿（MG-L）的总体平均回收率分别为93%和87%。在5至100 ppb的强化水平下，肌肉中MG-C和MG-L的总体平均回收率分别为85%和95%。所有强化水平下回收率的相对标准偏差（RSD），血浆为3.9%至7.0%，肌肉为2.1%至5.2%。该方法应用于鲶鱼在水体暴露于[14C]MG-C后采集的组织中的残留。在整个提取和净化过程中，血浆和肌肉中总放射性残留物的平均回收率分别为88%和87%，MG-C和MG-L的相应RSD与强化组织的RSD处于同一范围。MG-L被确认为鲶鱼中MG-C的主要代谢物。
