A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250 mm × 4.6 mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333 nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 and N-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15 M SDS-6% (v/v)-pentanol-0.01 M 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 and 1-naphthol, resp.), and limit of quantification (15 and 50 ng mL−1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.
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机译：已经开发出了一种液相色谱法，用于使用胶束流动相的C18色谱柱（250 mm×4.6 mm）和最大激发激发下的荧光检测法测定甲萘威，苯基-N-甲基氨基甲酸酯及其主要代谢物1-萘酚。 /发射波长分别为225/333 nm。在优化步骤中，考虑使用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。选择的流动相为pH 3缓冲的0.15 M SDS-6％（v / v）-戊醇-0.01 M NaH2PO4，根据ICH Tripartite准则，验证研究包括线性（r> 0.999），检测限（5甲萘威和1-萘酚的浓度分别为18 ng mL-1和18 ng mL-1，以及甲萘威和萘酚的定量限分别为15和50ng ng-1，且日内和日间精度均低于1 ％，而稳健性参数低于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。
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