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一步提取法气相色谱法-火焰光度检测法测定中药保健酒中 18 种有机磷农药残留量

One-step extraction for gas chromatography with flame photometric detection of 18 organophosphorus pesticides in Chinese medicine health wines.

机构信息

Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing 100193, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Feb 15;885-886:90-6. doi: 10.1016/j.jchromb.2011.12.019. Epub 2012 Jan 6.

Abstract

An easy, rapid and selective gas chromatography with flame photometric detection (GC-FPD) method was established for simultaneously determining 18 organophosphorus pesticides (OPPs) in 80 Chinese medicine (CM) health wines. This method was based on a simple one-step extraction procedure using a little solvent without any further cleanup steps. The optimized extraction solvent for the pesticides is acetone:dichloromethane (1:1, V/V) with extraction recovery of 79.0-109.1% and relative standard deviation (RSD) of 0.36-12.68%, respectively. The limits of detection (LODs) of the established GC-FPD method for all investigated pesticides ranged from 1 to 15ngmL(-1) and limits of quantification (LOQs) from 4 to 50ngmL(-1). Out of all 80 CM health wines, 18 OPPs were found in 8 samples at low concentrations of 8.2-37.9ngmL(-1). These pesticides were successfully confirmed by GC-MS. This is the first report of determining OPPs in CM health wines, providing references for monitoring the quality of CM health wine in routine analysis.

摘要

建立了一种简单、快速、选择性的气相色谱-火焰光度检测(GC-FPD)方法,用于同时测定 80 种中药保健酒中的 18 种有机磷农药(OPPs)。该方法基于使用少量溶剂的简单一步提取程序,无需进一步的净化步骤。优化的农药提取溶剂为丙酮:二氯甲烷(1:1,V/V),提取回收率为 79.0-109.1%,相对标准偏差(RSD)为 0.36-12.68%。所建立的 GC-FPD 方法对所有研究农药的检测限(LODs)范围为 1-15ngmL(-1),定量限(LOQs)范围为 4-50ngmL(-1)。在 80 种中药保健酒中,有 8 种样品中检出低浓度的 8.2-37.9ngmL(-1)的 18 种 OPPs。这些农药通过 GC-MS 成功确证。这是首次报道测定中药保健酒中的 OPPs,为常规分析中监测中药保健酒质量提供了参考。

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