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采用在线预富集的液相色谱法测定地表水中的杀菌剂异菌脲。

Liquid chromatographic determination of the fungicide iprodione in surface water, using on-line preconcentration.

作者信息

Goewie C E, Hogendoorn E A

出版信息

Sci Total Environ. 1985 Dec;47:349-60. doi: 10.1016/0048-9697(85)90341-9.

DOI:10.1016/0048-9697(85)90341-9
PMID:4089606
Abstract

A new method for on-line sample preparation of surface water extracts for the reversed phase HPLC analysis of the fungicide iprodione at the ppb level is presented. Water samples are extracted with dichloromethane and after concentration and evaporation to dryness, taken up in a mixture of acetonitrile/water. 2-Ml aliquots are injected onto a small precolumn, which is subsequently flushed with 20% acetonitrile in water as a clean-up step. The precolumn is switched on-line with the analytical column, and, using 47.5% acetonitrile in water as the eluent, the concentrated zone of iprodione is desorbed and transported to the analytical column. Detection takes place with UV at 229 nm. The resulting chromatograms are free of interferences. The detection limit of the method in 0.02 ppb. Good reproducibility and linear calibration curves are obtained. The results of the method are in agreement with those of capillary GC analysis with cold-on-column injection. The advantage of the method compared to GC is the lower susceptibility to errors due to the presence of interferences.

摘要

本文介绍了一种在线样品前处理方法,用于对地表水提取物进行反相高效液相色谱分析,以测定痕量水平的杀菌剂异菌脲。水样用二氯甲烷萃取,浓缩并蒸发至干后,用乙腈/水混合溶液复溶。取2 ml 等分试样注入小型预柱,随后用20%乙腈水溶液冲洗预柱作为净化步骤。预柱与分析柱在线切换,以47.5%乙腈水溶液作为洗脱液,将异菌脲浓缩区解吸并转移至分析柱。在229 nm处用紫外检测器进行检测。所得色谱图无干扰。该方法的检测限为0.02 ppb。获得了良好的重现性和线性校准曲线。该方法的结果与冷柱头进样毛细管气相色谱分析结果一致。与气相色谱相比,该方法的优点是对干扰物存在引起的误差敏感性较低。

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