Yang Fei, Bian Zhaoyang, Chen Xiaoshui, Liu San San, Liu Yang, Tang Gangling
China National Tobacco Quality Supervision and Test Center, Zhengzhou, 450000, People's Republic of China.
J AOAC Int. 2013 Sep-Oct;96(5):1134-7. doi: 10.5740/jaoacint.12-467.
A new method for determination of phenoxy acid herbicide residues in tobacco based on the use of liquid extraction/partition and dispersive SPE followed by HPLC/electrospray ionization-MS/MS is reported. Formic acid (2%, v/v) in acetonitrile as the extraction solvent and inclusion of citrate buffer helped partitioning of all analytes into the acetonitrile phase. Quantitative analysis was done in the multiple-reaction monitoring mode using two combinations of selected precursor ion and product ion transition for each compound. The recoveries obtained for each pesticide ranged between 85 and 110% at two spike concentration levels. Good linear relationships were observed, with the correlation coefficient (r2) >0.998 for all analytes. The method is simple, efficient, and sensitive, and each of its performance characteristics meets the requirements for determination of phenoxy acid herbicide residues in tobacco.
报道了一种基于液液萃取/分配和分散固相萃取，随后进行高效液相色谱/电喷雾电离-串联质谱法测定烟草中苯氧羧酸类除草剂残留的新方法。乙腈中2%（v/v）的甲酸作为萃取溶剂，加入柠檬酸盐缓冲液有助于将所有分析物分配到乙腈相中。采用多反应监测模式进行定量分析，每种化合物使用选定的前体离子和产物离子跃迁的两种组合。在两个加标浓度水平下，每种农药的回收率在85%至110%之间。观察到良好的线性关系，所有分析物的相关系数（r2）>0.998。该方法简单、高效、灵敏，其各项性能指标均符合烟草中苯氧羧酸类除草剂残留量测定的要求。
