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使用硅胶柱净化和带紫外检测的液相色谱法测定低水分粮食作物中的百草枯和敌草快。

Determination of paraquat and diquat in low-moisture food crops using silica column cleanup and liquid chromatography with UV detection.

作者信息

Chichila T M, Gilvydis D M

机构信息

U.S. Food and Drug Administration, Pesticides and Industrial Chemicals Research Center, Detroit, MI 48207.

出版信息

J AOAC Int. 1993 Nov-Dec;76(6):1323-8.

PMID:8286972
Abstract

A sample cleanup method was developed for the determination of paraquat (PQ) and diquat (DQ) in low-moisture food crops. Low-moisture commodities, such as milled dry navy beans, are digested in acid. PQ and DQ are isolated from the digestates by using a 4 g column of preconditioned silica gel. The analytes are concentrated and then determined by liquid chromatography with a silica analytical column, sodium chloride as an ion-pairing re-agent, and acetonitrile as an organic modifier. PD and DQ are determined simultaneously with a diode array UV absorbance detector. Recoveries for PQ and DQ were determined on 3 different fortified low-moisture crops. Fortification levels ranged from 0.01 to 0.30 ppm; average recoveries ranged from 47.5% (DQ) to 95.3% (PQ).

摘要

开发了一种用于测定低水分粮食作物中百草枯(PQ)和敌草快(DQ)的样品净化方法。低水分商品,如磨碎的干海军豆,用酸进行消化。通过使用4克预处理硅胶柱从消化物中分离出PQ和DQ。将分析物浓缩,然后用硅胶分析柱、氯化钠作为离子对试剂和乙腈作为有机改性剂的液相色谱法进行测定。使用二极管阵列紫外吸收检测器同时测定PQ和DQ。在3种不同加标低水分作物上测定了PQ和DQ的回收率。加标水平为0.01至0.30 ppm;平均回收率为47.5%(DQ)至95.3%(PQ)。

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