Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China.
J Agric Food Chem. 2012 Apr 25;60(16):4026-33. doi: 10.1021/jf205351t. Epub 2012 Apr 13.
A method for analysis of 37 pesticide residues in tea samples was developed and validated and was based on reversed-dispersive solid-phase extraction (r-DSPE) cleanup in acetonitrile solution, followed by liquid chromatography-electrospray tandem mass spectrometry determination. Green tea, oolong tea, and puer tea were selected as matrixes and represent the majority of tea types. Acetonitrile was used as the extraction solvent, with sodium chloride and magnesium sulfate enhancing partitioning of analytes into the organic phase. The extract was then cleaned up by r-DSPE using a mixture of multiwalled carbon nanotubes, primary secondary amine, and graphitized carbon black as sorbents to absorb interferences. Further optimization of sample preparation and determination allowed recoveries of between 70% and 111% for all 37 pesticides with relative standard deviations lower than 14% at two concentration levels of 10 and 100 μg kg(-1). Limits of quantification ranged from 5 to 20 μg kg(-1) for all pesticides. The developed method was successfully applied to the determination of pesticide residues in market tea samples.
建立并验证了一种分析茶叶样品中 37 种农药残留的方法。该方法基于反分散固相萃取(r-DSPE)在乙腈溶液中的净化,随后采用液相色谱-电喷雾串联质谱法测定。绿茶、乌龙茶和普洱茶被选为基质,代表了大多数茶类。乙腈被用作提取溶剂,氯化钠和硫酸镁增强了分析物向有机相的分配。然后,采用多壁碳纳米管、伯仲胺和石墨化炭黑的混合物通过 r-DSPE 对提取物进行净化,以吸收干扰物。通过进一步优化样品制备和测定条件,所有 37 种农药的回收率在 70%至 111%之间,两个浓度水平(10 和 100μg/kg)下的相对标准偏差均低于 14%。所有农药的定量限范围为 5 至 20μg/kg。该方法成功应用于市场茶叶样品中农药残留的测定。