School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, P. R. China.
J Sep Sci. 2011 Jan;34(2):202-9. doi: 10.1002/jssc.201000590. Epub 2010 Dec 7.
This paper described a simple, rapid and efficient method for the determination of N-methyl carbamate pesticides in tomato, cucumber, carrot and lettuce samples by dispersive liquid-liquid microextraction coupled with HPLC-diode array detection. Some experimental parameters that influenced the extraction efficiency, such as types and volumes of extraction and disperser solvents, extraction time and salt effect were examined and optimized. Under optimum conditions, the LOD of the method were 0.5-3.0 μg/kg depending on the compounds and the kind of vegetables. The linearities of the method were obtained in the range of 10.0-300 μg/kg for aldicarb, MTMC, carbofuran and carbaryl, and 20.0-600 μg/kg for isoprocarb, with the correlation coefficients ranging from 0.9921 to 0.9993. The RSD varied from 2.9 to 7.5% (n=5). The recoveries of the method for the five carbamates from vegetable samples at two different spiking levels were ranged from 77.8 to 98.2%. Results showed that the method we proposed can meet the requirements for the determination of N-methyl carbamate in vegetable samples and was finally applied to the analysis of target pesticides in vegetable samples taken from local markets.
本文描述了一种通过分散液-液微萃取结合高效液相色谱-二极管阵列检测法测定番茄、黄瓜、胡萝卜和生菜样品中 N-甲基氨基甲酸酯类农药的简单、快速、高效的方法。考察并优化了影响萃取效率的一些实验参数,如萃取和分散溶剂的种类和体积、萃取时间和盐效应。在最佳条件下,该方法的检出限(LOD)为 0.5-3.0μg/kg,具体取决于化合物和蔬菜的种类。该方法对涕灭威、灭多威、克百威和西维因的线性范围为 10.0-300μg/kg,异丙威的线性范围为 20.0-600μg/kg,相关系数范围为 0.9921-0.9993。相对标准偏差(RSD)为 2.9-7.5%(n=5)。该方法对两种不同添加水平下蔬菜样品中五种氨基甲酸酯的回收率为 77.8-98.2%。结果表明,该方法可满足蔬菜样品中 N-甲基氨基甲酸酯测定的要求,并最终应用于当地市场采集的蔬菜样品中目标农药的分析。