粮食中绿麦隆残留量的气相色谱分析
GAS CHROMATOGRAPHIC ANALYSIS OF CHLOROTOLURON RESIDUE IN GRAINS
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摘要: 本文用六氟丁酸酐直接衍生化气相色谱法测定粮食中绿麦隆农药残留量.粮食样品用甲醇-水提取.滤液用二氯甲烷或三氯甲烷-石油醚混合溶剂萃取,经硅镁吸附剂净化.以丙酮-石油醚为洗脱剂,洗脱液浓缩后用七氟丁酸酐直接衍生化,采用气相色谱法,电子捕获检测器测定.方法的线性范围为0—2.5μg·ml-1.对5g粮食样品,方法检出限为0.01mg·kg-1.对于小麦、玉米和大豆样品,加标回收率为82.4—91.2%,相对标准偏差为4.1—10.3%.对实际样品的测定和有关单位验证的结果表明,本方法适合于粮食中绿麦隆残留量的测定.Abstract: A method for determination of Chlorotoluron residue in grains by gas chromatogra-phy was developed.The grain sample was extracted with methanol-water (3:2).The filtrate was re-extracted with dichloromethane-petroleum (3.5:6.5) for maize and soybean, with tricholoromethane-petroleum (3.5:6.5) for wheat.The extract was cleaned up on a florisil column and followed by analysis with GC/ECD.The linear range of the method was 0-2.5μg·ml-1.The detection limit was 0.01mg·kg-1 for a grain sample of 5g.The recoveries of spiked samples ranged from 82.4-91.2% with the relative deviation standard of 4.1-10.3%.This method was experimentally verified by the relevant departments and the application in determination of grain samples showed that this method was sensitive, reliable and suitable for analysis of Chlorotoluron residue in grains.
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Key words:
- Chlorotoluron /
- analysis of pesticide residue /
- grain /
- gas chromatography
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