Worobey B L, Shields J B
Health and Welfare Canada, Food Research Division, Ottawa, Ontario.
J Assoc Off Anal Chem. 1989 Mar-Apr;72(2):368-71.
A new method is described for the determination of the herbicide fluazifop-butyl, and its metabolite fluazifop acid, in soybeans and soybean oil as fluazifop acid. Liquid chromatography with amperometric detection (LC/AD) is used to determine fluazifop acid produced from the metabolism or base hydrolysis of fluazifop-butyl in soybeans and soybean oil. These foods were spiked with fluazifopbutyl at 0.05, 0.10, and 0.50 ppm and hydrolyzed with 0.2N NaOH in methanol. The hydrolysate (adjusted to pH less than or equal to 1) is extracted with dichloromethane and the extract is washed with 1.0% NaHCO3. The NaHCO3 is acidified to pH less than or equal to 1 and extracted with dichloromethane; the partitioning is repeated 2 more times. The dichloromethane is removed, mobile phase solvent is added, and aliquots are injected onto a PRP-1 liquid chromatographic column; fluazifop acid is separated from coextracted compounds and detected at an applied potential of + 1.25 V, using an amperometric electrochemical detector in the oxidation mode. Recoveries ranged from 69 +/- 6.5 to 101 +/- 18% and from 72 +/- 7.5 to 88 +/- 11% for soybeans and soybean oil, respectively. Accuracy of these recoveries was confirmed by use of 14C-radiolabeled fluazifop-butyl and by liquid scintillation spectrometry of the 14C-fluazifop acid released.
本文描述了一种测定大豆和大豆油中除草剂精稳杀得及其代谢物精稳杀得酸的新方法。采用液相色谱 - 安培检测法（LC/AD）测定大豆和大豆油中精稳杀得经代谢或碱水解生成的精稳杀得酸。向这些食品中添加浓度为0.05、0.10和0.50 ppm的精稳杀得，并用0.2N氢氧化钠的甲醇溶液进行水解。将水解产物（调节至pH小于或等于1）用二氯甲烷萃取，萃取液用1.0%的碳酸氢钠洗涤。将碳酸氢钠酸化至pH小于或等于1，再用二氯甲烷萃取；该分配过程重复两次。去除二氯甲烷，加入流动相溶剂，取 aliquots 注入PRP - 1液相色谱柱；使用安培电化学检测器在氧化模式下，于 + 1.25 V的施加电位下将精稳杀得酸与共萃取化合物分离并检测。大豆和大豆油的回收率分别为69 ± 6.5%至101 ± 18%和72 ± 7.5%至88 ± 11%。通过使用14C - 放射性标记的精稳杀得以及对释放的14C - 精稳杀得酸进行液体闪烁光谱分析，证实了这些回收率的准确性。 （注：aliquots未找到准确对应的中文词汇，可根据上下文理解为“等分试样”等，这里保留英文）
