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采用带电子捕获检测器的气相色谱法对大米和土壤样品中敌稗残留量进行测定与验证

Estimation and Validation of Propanil Residues in Rice and Soil Samples by Gas Liquid Chromatography with Electron Capture Detector.

作者信息

Sandhu Amanpal Kaur, Mandal Kousik, Singh Balwinder

机构信息

Pesticide Residue Analysis Laboratory, Department of Entomology, Punjab Agricultural University, Ludhiana, 141004, Punjab, India.

出版信息

Bull Environ Contam Toxicol. 2015 Sep;95(3):368-72. doi: 10.1007/s00128-015-1610-9. Epub 2015 Aug 1.

Abstract

The purpose of this analysis was to develop an efficient analysis for the estimation of residues of propanil in rice grain, husk, straw and soil samples. A liquid-liquid partitioning method was used for the extraction of propanil residues from the rice grains and its contents. For this, representative 10 g samples of blended rice grain, husk, straw and soil were soaked in acetone for 24 h, and the contents then partitioned two times into 100 and 50 mL dichloromethane and one time with 100 mL hexane. The combined organic layers were collected and were concentrated to 10 mL acetone using a rotary vacuum evaporator at 40°C. The extract was then subjected to cleanup by dispersive solid phase extraction. The final extract was injected onto a GLC column, where the propanil residues were determined by electron capture detector. The percentage recoveries were ranged from 84.9 % to 98.3 % when samples were spiked at the levels of 0.05, 0.25 and 0.50 mg/kg. The limits of quantification and detection were 0.05 and 0.017 mg/kg, respectively.

摘要

本分析的目的是开发一种高效的分析方法,用于估算水稻籽粒、稻壳、稻草和土壤样品中敌稗的残留量。采用液-液分配法从水稻籽粒及其内容物中提取敌稗残留量。为此,将10克具有代表性的混合水稻籽粒、稻壳、稻草和土壤样品在丙酮中浸泡24小时,然后将内容物分两次用100毫升和50毫升二氯甲烷进行分配,并用100毫升己烷进行一次分配。收集合并的有机层,并在40℃下使用旋转真空蒸发器浓缩至10毫升丙酮。然后通过分散固相萃取对提取物进行净化。将最终提取物注入气相色谱柱,通过电子捕获检测器测定敌稗残留量。当样品添加水平为0.05、0.25和0.50毫克/千克时,回收率在84.9%至98.3%之间。定量限和检测限分别为0.05和0.017毫克/千克。

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