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福美双及其在干粉剂配方中低毒转化产物的分离与同步液相色谱分析

Isolation and simultaneous LC analysis of thiram and its less toxic transformation product in DS formulation.

作者信息

Walia Suresh, Sharma Rajendra Kumar, Parmar Balraj S

机构信息

Division of Agricultural Chemicals, Indian Agricultural Research Institute, New Delhi, 110012, India.

出版信息

Bull Environ Contam Toxicol. 2009 Sep;83(3):363-8. doi: 10.1007/s00128-009-9754-0. Epub 2009 May 19.

Abstract

A simple and sensitive high pressure liquid chromatographic method has been developed for the simultaneous determination of Thiram and its transformation product using isocratic mixture of methanol-water (65:35) at flow rates of 0.75 mL min(-1), PDA detector using UV absorbance (lambda(max)) at 217 nm for Thiram and 265.5 nm for the transformation product. The transformation product was isolated from the commercial DS formulation and has been tentatively assigned the structure by (1)H NMR and ESI-MS spectral data. The separation is dependent on the nature of the mobile phase, its flow rate and the nature of the HPLC column. The detection limit (signal/noise; S/N = 3) for both Thiram and its transformation product was 0.2 ppm. The method has been successfully applied to analysis of soil and soybean samples spiked with Thiram, its transformation product and a commercial sample containing these products.

摘要

已开发出一种简单且灵敏的高效液相色谱法,用于同时测定福美双及其转化产物。该方法采用甲醇 - 水(65:35)等度混合液,流速为0.75 mL min⁻¹,使用光电二极管阵列(PDA)检测器,在217 nm处检测福美双的紫外吸光度(λmax),在265.5 nm处检测转化产物的紫外吸光度。从市售的DS制剂中分离出了转化产物,并通过¹H NMR和电喷雾电离质谱(ESI-MS)光谱数据初步确定了其结构。分离取决于流动相的性质、流速以及高效液相色谱柱的性质。福美双及其转化产物的检测限(信号/噪声;S/N = 3)均为0.2 ppm。该方法已成功应用于分析添加了福美双及其转化产物的土壤和大豆样品,以及含有这些产物的商业样品。

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