Worobey B L, Shields J B
Health and Welfare Canada, Food Research Division, Ottawa, Ontario.
J Assoc Off Anal Chem. 1987 Nov-Dec;70(6):1021-4.
A new method is described for the determination of the herbicide naptalam and its metabolite 1-naphthylamine in several foods. The method is sensitive, selective, and extremely rapid compared with previously reported methods. Liquid chromatography with electrochemical detection (LC/ECD) is used to determine 1-naphthylamine produced from the metabolism or base hydrolysis of naptalam in asparagus, peaches, and cranberries. These foods were spiked with naptalam at 0.05 and 0.11 ppm and hydrolyzed with 30% NaOH with concomitant distillation of 1-naphthylamine. Aliquots of the distillate were injected onto a reverse-phase PRP-1 LC column for separation of 1-naphthylamine from coextractives near the solvent front and detection at an applied potential of +0.83 V using an amperometric electrochemical detector in the oxidation mode. Recoveries ranged from 89% +/- 2% to 97% +/- 8% for all foods at both spiking levels. Accuracy of these recoveries was confirmed by use of 14C-radiolabeled naptalam and radioassay by liquid scintillation spectrometry of the 14C-1-naphthylamine released.
描述了一种测定几种食品中除草剂萘草胺及其代谢物1-萘胺的新方法。与先前报道的方法相比，该方法灵敏、有选择性且极其快速。采用液相色谱-电化学检测法（LC/ECD）测定芦笋、桃子和蔓越莓中萘草胺经代谢或碱水解产生的1-萘胺。这些食品添加了浓度为0.05 ppm和0.11 ppm的萘草胺，并用30%氢氧化钠水解，同时蒸馏出1-萘胺。取蒸馏液的等分试样注入反相PRP-1液相色谱柱，以从溶剂前沿附近的共提取物中分离出1-萘胺，并使用安培电化学检测器在氧化模式下于+0.83 V的施加电位下进行检测。在两个加标水平下，所有食品的回收率范围为89%±2%至97%±8%。通过使用14C放射性标记的萘草胺以及对释放出的14C-1-萘胺进行液体闪烁光谱法放射性测定，证实了这些回收率的准确性。
