Krause R T
Division of Contaminants Chemistry, Food and Drug Administration, Washington, DC 20204.
J Chromatogr. 1988 Jun 17;442:333-43. doi: 10.1016/s0021-9673(00)94481-9.
A high-performance liquid chromatographic technique is reported which selectively detects the phenolic moiety of aryl N-methylcarbamates at low nanogram levels. The carbamates are separated on a C-8 column using an acetonitrile-water gradient mobile phase. The eluted carbamates are hydrolyzed in-line by post-column addition of base, which also serves as electrolyte in the electrochemical (coulometric) detection of the resulting phenols. The technique was tested with six carbamates (bufencarb, carbaryl, carbofuran, 3-hydroxycarbofuran, isoprocarb and methiocarb) and four crops (apples, cabbage, grapes and tomatoes). Optimum detector responses and stability for the carbamates were attained at 0.60 V. Detector response to the carbamates in the presence of crop coextractives was 99% of theoretical with a standard deviation of 2.8% at the 0.05- to 0.1-ppm fortification level. The lower limit of quantitation is 0.01 ppm. Other electrochemical detectors were evaluated for suitability for this work.
报道了一种高效液相色谱技术，该技术能在低纳克水平下选择性检测芳基N - 甲基氨基甲酸酯的酚基部分。氨基甲酸酯在C - 8柱上进行分离，使用乙腈 - 水梯度流动相。洗脱后的氨基甲酸酯通过柱后添加碱进行在线水解，碱在所得酚类的电化学（库仑）检测中也用作电解质。该技术用六种氨基甲酸酯（丁硫克百威、西维因、克百威、3 - 羟基克百威、异丙威和甲硫威）和四种作物（苹果、卷心菜、葡萄和西红柿）进行了测试。在0.60 V时，氨基甲酸酯达到了最佳检测器响应和稳定性。在0.05至0.1 ppm强化水平下，在作物共提取物存在的情况下，检测器对氨基甲酸酯的响应为理论值的99%，标准偏差为2.8%。定量下限为0.01 ppm。还评估了其他电化学检测器对此工作的适用性。
