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采用改进的QuEChERS萃取法和高效液相色谱/串联质谱法测定烟草中的氯苯氧基酸类除草剂

Determination of chlorinated phenoxy acid herbicides in tobacco by modified quechERS extraction and high-performance liquid chromatography/tandem mass spectrometry.

作者信息

Yang Fei, Bian Zhaoyang, Chen Xiaoshui, Liu San San, Liu Yang, Tang Gangling

机构信息

China National Tobacco Quality Supervision and Test Center, Zhengzhou, 450000, People's Republic of China.

出版信息

J AOAC Int. 2013 Sep-Oct;96(5):1134-7. doi: 10.5740/jaoacint.12-467.

Abstract

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.

摘要

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。

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