A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and itsmain metabolite 1-naphthol, using a C18 column (250mm×4.6mm) with a micellar mobile phase and fluorescence detectionat maximum excitation/emission wavelengths of 225/333 nm, respectively. In the optimization step, surfactants sodium dodecylsulphate (SDS), Brij-35 and N-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol wereconsidered. The selected mobile phase was 0.15M SDS-6% (v/v)-pentanol-0.01M NaH2PO4 buffered at pH 3. Validation studies,according to the ICH Tripartite Guideline, included linearity (r > 0.999), limit of detection (5 and 18 ng mL−1, for carbaryl and1-naphthol, resp.), and limit of quantification (15 and 50 ng mL−1, for carbaryl and 1-naphthol, resp.), with intra- and interdayprecisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routineanalysis of these two compounds in water, soil, and vegetables samples.
展开▼
机译：已开发出一种液相色谱法，用于测定碳酰芳基，苯基-N-甲基氨基甲酸酯及其主要代谢物1-萘酚，该方法使用具有胶束流动相的C18色谱柱（250mm×4.6mm）和在最大激发/发射波长下进行荧光检测分别为225/333 nm。在优化步骤中，考虑了表面活性剂十二烷基硫酸钠（SDS），Brij-35和N-鲸蜡基吡啶鎓一水合物，以及有机溶剂丙醇，丁醇和戊醇。选择的流动相是在pH 3缓冲的0.15M SDS-6％（v / v）-戊醇-0.01M NaH2PO4，根据ICH Tripartite准则进行的验证研究包括线性（r> 0.999），检测极限（5甲萘威和1-萘酚分别为18 ng mL-1和定量限（甲萘威和1-萘酚分别为15和50 ng mL-1），日内和日间精密度均低于1％，鲁棒性参数低于3％。结果表明该方法足以常规分析水，土壤和蔬菜样品中的这两种化合物。
展开▼
