Lynch M J, Bartolucci S R
J Assoc Off Anal Chem. 1982 Mar;65(2):227-33.
A gas-liquid chromatographic assay has been developed to determine major residues of morantel in bovine liver, a target tissue, at levels of 0.2-0.8 ppm. The method is based on hydrolysis of the N-methyltetrahydropyrimidine portion of morantel and its metabolites to N-methyl-1,3-propanediamine, and conversion of the diamine to an N,N'-bis-(2-nitro-4-trifluoromethylphenyl) derivative. The addition of an internal standard, N-ethyl-1,3-propanediamine, to the tissue sample circumvents any potential problem that could arise from variable reaction yields, and eliminates the true recovery as a factor affecting the accuracy and precision of the procedure. The concentrations of the derivatives are determined by pulsed electron capture gas-liquid chromatography over a linear dynamic range equivalent to 0.2-0.8 ppm morantel. The method has been evaluated at 0, 0.2, 0.4, and 0.8 ppm levels in fortified bovine liver, and in a withdrawal sample containing physiologically incurred morantel residues. Mean values of 0.22 +/- 0.015, 0.40 +/- 0.033, and 0.79 +/- ppm were found for fortified samples, 0.02 ppm for control liver, and 0.56 +/- 0.050 ppm for the withdrawal sample.
已开发出一种气液色谱分析法，用于测定牛肝脏（一种靶组织）中噻嘧啶的主要残留量，残留水平为0.2 - 0.8 ppm。该方法基于将噻嘧啶及其代谢物的N - 甲基四氢嘧啶部分水解为N - 甲基 - 1,3 - 丙二胺，并将二胺转化为N,N'-双-(2 - 硝基 - 4 - 三氟甲基苯基)衍生物。向组织样品中添加内标物N - 乙基 - 1,3 - 丙二胺，可避免因反应产率变化可能产生的任何潜在问题，并消除了实际回收率这一影响该方法准确性和精密度的因素。通过脉冲电子捕获气液色谱法在相当于0.2 - 0.8 ppm噻嘧啶的线性动态范围内测定衍生物的浓度。该方法已在添加了噻嘧啶的牛肝脏中0、0.2、0.4和0.8 ppm水平下以及在含有生理产生的噻嘧啶残留的停药样品中进行了评估。添加样品的平均值为0.22±0.015、0.40±0.033和0.79±ppm，对照肝脏为0.02 ppm，停药样品为0.56±0.050 ppm。
