Turnipseed S B, Roybal J E, Hurlbut J A, Long A R
U.S. Food and Drug Administration, Denver Federal Center, CO 80225-0087, USA.
J AOAC Int. 1995 Jul-Aug;78(4):971-7.
A gas chromatographic/mass spectrometric (GC/MS) method was developed to confirm the presence of leucomalachite green (LMG), a metabolite of the triphenylmethane dye malachite green (MG), in catfish tissue. Residues were isolated according to a previously described liquid chromatographic (LC)/VIS spectrometric analysis of MG and LMG in fish. In our isolation procedure, analytes are extracted from tissue with acetonitrile-buffer, partitioned into CH2Cl2, and applied to neutral alumina and propylsulfonic acid solid-phase extraction cartridges. Before GC/MS analysis, extracts prepared for the LC determinative method are eluted from a cyano solid-phase extraction cartridge, extracted into organic solvent, and concentrated for GC/MS analysis. Selected ion monitoring was performed by using 5 diagnostic ions (m/z 330, 329, 253, 210, and 165) of LMG. The method was validated by confirming LMG in tissue fortified with mixtures of MG and LMG (5 and 10 ng/g each) and in tissue from fish that had been exposed to low levels of MG.
开发了一种气相色谱/质谱（GC/MS）方法，用于确认鲶鱼组织中是否存在无色孔雀石绿（LMG），它是三苯甲烷染料孔雀石绿（MG）的一种代谢物。根据先前描述的鱼类中MG和LMG的液相色谱（LC）/可见光谱分析方法分离残留物。在我们的分离过程中，用乙腈缓冲液从组织中提取分析物，分配到二氯甲烷中，然后应用于中性氧化铝和丙基磺酸固相萃取柱。在进行GC/MS分析之前，将为LC测定方法制备的提取物从氰基固相萃取柱上洗脱，萃取到有机溶剂中，并浓缩用于GC/MS分析。通过使用LMG的5个诊断离子（m/z 330、329、253、210和165）进行选择离子监测。通过在添加了MG和LMG混合物（各5和10 ng/g）的组织以及暴露于低水平MG的鱼类组织中确认LMG，对该方法进行了验证。
