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[气相色谱法测定马铃薯、马铃薯叶和土壤中开乐凡及开蓬的方法提示]

[Methodological hints on the gas chromatographic determination of kelevan and kepone in potatoes, potato foliage and soil].

作者信息

Dabrowski J

出版信息

Nahrung. 1979;23(1):33-7. doi: 10.1002/food.19790230106.

Abstract

The gas chromatographic determination of Kelevan, an ethyllaevulinic acid derivative of Kepone, requires its conversion to Kepone. Thermal decomposition in the injection block of the gas chromatograph at 45 degrees C. has proved to be well suited for routine work. The sample is extracted with acetonitrile; the extract is purified and concentrated under reduced pressure. The separation of Kelevan from Kepone already metabolically produced is possible by column chromatography (silica gel; elution with benzene and 5% acetone in benzene). The determination of pre-existent Kepone and of Kelevan (after thermal conversion to Kepone) was achieved by means of a Pye-Unicam gas chromatograph. The limits of detection are 0.002 p.p.m. for Kepone, and 0.003 p.p.m. for Kelevan. The recovery of Kelevan and Kepone added to control samples (for every 10 determinations with different amounts added to potatoes, potato foliage and soil samples) ranges from 63 to 88%; the standard derivation, from +/- 1.7 to 7.3%.

摘要

开蓬的乙基乙酰丙酸衍生物克勒凡的气相色谱测定需要将其转化为开蓬。已证明在气相色谱仪的进样块中于45℃进行热分解非常适合常规工作。样品用乙腈萃取;萃取液经减压纯化和浓缩。通过柱色谱法(硅胶;用苯和5%苯中的丙酮洗脱)可以将已代谢产生的克勒凡与开蓬分离。通过派-尤尼坎气相色谱仪测定预先存在的开蓬和克勒凡(热转化为开蓬后)。检测限对于开蓬为0.002 ppm,对于克勒凡为0.003 ppm。添加到对照样品中的克勒凡和开蓬的回收率(对添加到土豆、土豆叶和土壤样品中的不同量进行每10次测定)为63%至88%;标准偏差为±1.7%至7.3%。

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