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[用于测定甲拌磷和倍硫磷的比较薄层色谱研究]

[Comparative thin-layer chromatographic studies for determining phorate and fenthion].

作者信息

Ignatov M

出版信息

Vet Med Nauki. 1977;14(3):39-44.

PMID:906307
Abstract

Experiments were carried out to use thin-layer chromatography to determine pure substances of the organic phosphorous insecticides forat and phenothion. Three sorbents were employed to establish the most appropriate conditions for the application of a fast, readily applicably and highly sensitive method--silica gel G, DG and Kiselgur "Merk", as well as 14 mobile phases--monocompound (n-hexane, n-heptane, acetone benzol and toluol), double combinations (hexane-acetone 4:1, hexane-acetone 9:1, hexane-benzol 1:1, hexane-benzol 4:1, heptane-acetone 7:1, benzol-hexane 4:1, benzol-acetone 9:1, and petrolium ether-tetrachlormethane) and triple combinations (acetone-toluol-hexane 1:15 and 5 developers (a diazosalt, bromine vapours + diazosalt, palladium bichloride, bromphenol blue, and silver nitrate, sodium hydroxide, ammonia gas). Established was the fact that the best results are obtained with the use of silica gel G, the mobile phase heptan-acetone 7:1, and the developer of 0.2% solution of palladium bichloride in 0.5 per cent solution of hydrochloric acid. In chromatogrammes the forat compound appears as a tile red portion with a darker peripheral part and Rf = 0.61, and phenothion--in yellow, with a brownish halo and Rf = 0.41. The method is highly sensitive--for forat 0.5 microgram, and for phenothion 0.5 microgram. In determining these insecticides it is possible to use as a sorbent silica gel "Merk" 1:1 with the same degree of sensitivity, but with higher Rf values.

摘要

开展了实验,以利用薄层色谱法测定有机磷杀虫剂伐灭磷和稻丰散的纯物质。使用了三种吸附剂来建立一种快速、易于应用且高度灵敏的方法的最合适条件——硅胶G、DG和默克硅胶“Merk”,以及14种流动相——单一组分(正己烷、正庚烷、丙酮、苯和甲苯)、双组合(己烷 - 丙酮4:1、己烷 - 丙酮9:1、己烷 - 苯1:1、己烷 - 苯4:1、庚烷 - 丙酮7:1、苯 - 己烷4:1、苯 - 丙酮9:1和石油醚 - 四氯化碳)和三组合(丙酮 - 甲苯 - 己烷1:15)以及5种显色剂(重氮盐、溴蒸气 + 重氮盐、二氯化钯、溴酚蓝和硝酸银、氢氧化钠、氨气)。结果表明,使用硅胶G、流动相庚烷 - 丙酮7:1以及0.2%二氯化钯在0.5%盐酸溶液中的显色剂可获得最佳结果。在色谱图中,伐灭磷化合物呈现为砖红色部分,周边颜色较深,比移值Rf = 0.61,稻丰散呈现为黄色,带有褐色光晕,Rf = 0.41。该方法高度灵敏——对伐灭磷为0.5微克,对稻丰散为0.5微克。在测定这些杀虫剂时,也可以使用默克硅胶“Merk”1:1作为吸附剂,灵敏度相同,但比移值更高。

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