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采用电子捕获检测的气液色谱法测定水中某些苯氧乙酸类除草剂以其2,2,2-三氯乙酯形式存在的残留量。

Gas-liquid chromatographic method with electron-capture detection for the determination of residues of some phenoxyacetic acid herbicides in water as their 2,2,2-trichloroethyl esters.

作者信息

Mierzwa S, Witek S

出版信息

J Chromatogr. 1977 Jun 1;136(1):105-11. doi: 10.1016/s0021-9673(00)82999-4.

Abstract

A gas-liquid chromatographic method with electron-capture detection was developed for the determination of residues of 2,4-dichlorophenoxyacetic acid (2,4-D) and 4-chloro-2-methylpenoxyacetic acid (MCPA) in water as their 2,2,2-trichloroethyl esters, and the sensitivity was compared with that for 2-chloro- and 2,2,2-trifluoroethyl esters. The residue is isolated by sorption of the phenoxy acid on Amberlite XAD-4, eluted with benzene and then esterified with 20% (v/v) 2,2,2-trichloroethanol in trifluoroacetic anhydride in the presence of sulphuric acid. The recoveries at the 0.4 ppb level are 92.1 +/- 3.4% (2,4-D) and 87.8 +/- 2.1% (MCPA) and the detection limits for a 1-1 sample of water are 0.096 ppb (2,4-D) and 0.06 ppb (MCPA).

摘要

建立了一种带电子捕获检测的气液色谱法,用于测定水中2,4-二氯苯氧乙酸(2,4-D)和4-氯-2-甲基苯氧乙酸(MCPA)的残留量,以其2,2,2-三氯乙酯形式存在,并将该方法的灵敏度与2-氯乙酯和2,2,2-三氟乙酯的灵敏度进行了比较。通过将苯氧酸吸附在Amberlite XAD-4上分离残留量,用苯洗脱,然后在硫酸存在下,于三氟乙酸酐中用20%(v/v)2,2,2-三氯乙醇进行酯化。0.4 ppb水平下的回收率分别为92.1±3.4%(2,4-D)和87.8±2.1%(MCPA),对于1升水样的检测限分别为0.096 ppb(2,4-D)和0.06 ppb(MCPA)。

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