Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, P. R. China.
J Sep Sci. 2011 Jan;34(2):210-6. doi: 10.1002/jssc.201000489. Epub 2010 Dec 6.
A multi-residue method for the analysis of pesticides in tea was developed by online size exclusion chromatography (SEC)-GC/MS with full scan mode. The sample was fortified with chlorpyrifos-d(10) isotope internal standard and extracted by acetonitrile. After purification by primary secondary amine sorbent and solvent exchange by SEC mobile phase, the sample was detected by online SEC-GC/MS. The purification result of the online system was evaluated by comparing the correlation between Chinese cabbage and tea matrix. The factors for method optimization included sample preparation, matrix effects and the instrument parameters of each online component. Scatter plot was introduced in this study to directly illustrate the results of the condition optimization and matrix effects in the online system. For most of the pesticides, the average recoveries ranged from 70 to 130% and the RSD were below 15%. The feasibility of the application of full scan mode in multi-residue determination of trace amounts of pesticides (LODs below 0.01 mg/kg) in a complex matrix was discussed.
建立了一种在线凝胶渗透色谱-气相色谱/质谱联用(SEC-GC/MS)全扫描模式分析茶叶中多种农药残留的方法。样品用毒死蜱-d10 同位素内标溶液提取,乙腈提取液经伯仲胺固相萃取柱净化和 SEC 流动相溶剂置换后,在线进样分析。通过对比甘蓝和茶叶基质的相关性,评估了在线净化系统的净化效果。方法优化的因素包括样品前处理、基质效应以及各个在线组件的仪器参数。本研究引入散点图,直观地说明了在线系统中条件优化和基质效应的结果。对于大多数农药,平均回收率在 70%至 130%之间,相对标准偏差(RSD)低于 15%。探讨了全扫描模式在复杂基质中痕量农药(LOD 低于 0.01mg/kg)多残留检测中的应用可行性。