薄层色谱-4-氨基安替比林-铁氰化钾体系光度法测定水杨硫磷的研究

Thin layer chromatography-catalytic spectrometric determination of trace salithion with 4-aminoantipyrne-potassium ferricyanide system

目的：建立了薄层色谱-4-氨基安替比林-铁氰化钾体系光度法测定水杨硫磷的方法。方法：用薄层层析分离杂质后,加甲醇萃取并用氢氧化钠溶液使其水解,得到的水解产物在碱性介质中与4-氨基安替比林-铁氰化钾生成络合物,于波长540 nm处,测定其吸光度,从而计算出水杨硫磷的含量。与此同时还研究了测定的缓冲溶液及pH范围,显色剂,增敏剂等对体系的影响。结果：方法的线性范围为2-10μg/ml。平行测定6次,分析了加标水果、蔬菜、水等样品,回收率和RSD分别为92.5%-102.5%,1.7%-3.2%之间。结论：该法简便、高效,适合各类样品中水杨硫磷的分析。

Objective：To establish a new catalytic spectrophotometric method for determination of trace Salithion based on the color reactions of 4-aminoantipyinc oxidized by potassium ferricyanide in potassium chloride-acid boron acid medium.Methods：The sample was separate by thin layer chromatography and the separateion was extracted with CH3OH,then Sodium Hydroxide was added.The hydrolyze product reacted with 4-aminoantipyrne-potassium ferricyanide in alkalinity medium.The experimental condition of system were optimized.Results：The liner ranges was from 2 to 10 μg/ml.Meanwhile,the recovery of standard addition was from 92.5% to 102.5% in the sample of fruit,vegetable and water.The RSD was from 1.7% to 3.2%.Conclusion：The method is used for the determination of trace Salthin in spiked tap water,vegetable and fruits etc.