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气动雾化-气固萃取白酒中部分农药残留。

Pneumatic nebulization gas-solid extraction of some pesticides in liquor.

机构信息

College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, China.

出版信息

J Chromatogr A. 2012 Aug 31;1253:11-5. doi: 10.1016/j.chroma.2012.06.099. Epub 2012 Jul 8.

Abstract

In general, solid phase extraction (SPE) was applied to the separation and concentration of analytes from liquid samples. However, the SPE generally cannot be applied directly to the separation and concentration of analytes from liquor in which the concentration of ethanol is high, because the ethanol can elute the analytes from the SPE column and the analytes can hardly been adsorbed onto the column. In the work, the pneumatic nebulization coupled with gas-solid extraction (PN-GSE) was applied to the extraction of several pesticides, including fenuron, chlortoluron, karmex, linuron and prebane, from liquor samples. The high concentration of ethanol in the liquor samples cannot elute the analytes from the SPE column. The high performance liquid chromatography was applied to the separation and determination of the analytes. Experimental parameters affecting the performances of PN-GSE, such as types and amount of packed material of the column, temperature of the spray chamber, flow rate of carrier gas, pumping rate of gas and volume of elution solvent were examined and optimized. The limits of detection for the analytes were in the range of 0.19-0.26 μg L⁻¹. Liquor samples were analyzed and the recoveries of the analytes in spiked samples were from 91.0 to 106.3%. The relative standard deviations were lower than 6.5%.

摘要

一般来说,固相萃取(SPE)用于从液体样品中分离和浓缩分析物。然而,SPE 通常不能直接用于从乙醇浓度高的酒样中分离和浓缩分析物,因为乙醇会从 SPE 柱中洗脱分析物,并且分析物很难被吸附到柱上。在这项工作中,气动雾化与气固萃取(PN-GSE)被用于从酒样中萃取几种农药,包括苯隆、绿麦隆、异丙隆、利谷隆和苯并呋喃。酒样中乙醇浓度高,不会从 SPE 柱中洗脱分析物。高效液相色谱法用于分析物的分离和测定。考察并优化了影响 PN-GSE 性能的实验参数,如柱的填充材料的类型和用量、喷雾室温度、载气流速、气体抽提速率和洗脱溶剂的体积。分析物的检出限在 0.19-0.26μg/L 范围内。对加标酒样进行了分析,分析物的回收率在 91.0%至 106.3%之间。相对标准偏差低于 6.5%。

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