Roybal J E, Pfenning A P, Munns R K, Holland D C, Hurlbut J A, Long A R
U.S. Food and Drug Administration, Animal Drugs Research Center, Denver Federal Center, CO 80225-0087, USA.
J AOAC Int. 1995 Mar-Apr;78(2):453-7.
To determine residues of malachite green (MG) and its metabolite, leucomalachite green (LMG), in catfish tissue, analytes are extracted with acetonitrile-buffer and the extract is partitioned into methylene chloride. Final cleanup and isolation are performed on neutral alumina solid-phase extraction (SPE) and propylsulfonic acid cation-exchange SPE columns before analysis by liquid chromatography with visible detection. PbO2 postcolumn oxidation is performed by isocratic elution with a buffered mobile phase from a cyano column. Recoveries and relative standard deviations (RSDs) from fortified catfish tissues were 72.9% (RSD, 1.92%; 23 ppb), 75.5% (RSD, 6.85%; 11 ppb), and 69.6% (RSD, 6.93%; 5.7 ppb) for MG and 87.4% (RSD, 2.92%; 21 ppb), 88.1% (RSD, 5.94%; 10 ppb), and 82.6% (RSD, 11.5%; 5.3 ppb) for LMG. The method was applied to MG-incurred catfish at depuration times of 0, 2, 4, 8, and 24 h. Average levels of residual MG and LMG in the 24 h depuration catfish tissue were 73.4 and 289 ppb, respectively.
为测定鲶鱼组织中孔雀石绿(MG)及其代谢物隐色孔雀石绿(LMG)的残留量,用乙腈 - 缓冲液提取分析物,提取物再用二氯甲烷进行液液分配。在通过可见检测的液相色谱分析之前,最终的净化和分离在中性氧化铝固相萃取(SPE)柱和丙基磺酸阳离子交换SPE柱上进行。通过氰基柱用缓冲流动相进行等度洗脱来进行柱后PbO₂氧化。在添加了MG和LMG的鲶鱼组织中的回收率和相对标准偏差(RSD),MG分别为72.9%(RSD,1.92%;23 ppb)、75.5%(RSD,6.85%;11 ppb)和69.6%(RSD,6.93%;5.7 ppb),LMG分别为87.4%(RSD,2.92%;21 ppb)、88.1%(RSD,5.94%;10 ppb)和82.6%(RSD,11.5%;5.3 ppb)。该方法应用于净化时间为0、2、4、8和24小时的添加了MG的鲶鱼。在净化24小时的鲶鱼组织中,MG和LMG的平均残留水平分别为73.4和289 ppb。