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高效液相色谱法同时分析水和碱性土壤中的苯磺隆、甲磺隆和氯磺隆。

Simultaneous analysis of triasulfuron, metsulfuron-methyl and chlorsulfuron in water and alkaline soils by high-performance liquid chromatography.

作者信息

Sarmah A K, Kookana R S

机构信息

Cooperative Research Centre for Soil and Land Management, Glen Osmond, Australia.

出版信息

J Environ Sci Health B. 1999 May;34(3):363-80. doi: 10.1080/03601239909373203.

Abstract

A method capable of simultaneously detecting residues of three sulfonylurea herbicides at microgram/l and microgram/kg level in water and alkaline soils has been described. The method is based on solid phase extraction and HPLC with UV detection. In alkaline soils especially those containing low organic carbon it was possible to extract the herbicides with de-ionised water and no clean up step was needed. Soil samples spiked with technical grade triasulfuron, metsulfuron-methyl and chlorsulfuron were extracted twice by shaking with de-ionised water for one hour and centrifuging at 10,000 rpm for 15 minutes. Supernatants filtered through glass micro-fibre filters were passed through C18 cartridges previously pre-conditioned with methanol and de-ionised water at a flow rate of < 20 ml/min. Residues of the herbicides retained on the cartridge were eluted with acidified methanol. The eluate was analysed by HPLC. A C18 column was used with a mobile phase of methanol/water (40 + 60, V/V for for the herbicide residues were 1.0 microgram/l and 3 micrograms/kg in water and soil, respectively. The average recoveries for water samples ranged from 73-94%, while for soil samples recoveries were 77-97% for the three compounds studied.

摘要

已描述了一种能够同时检测微克/升和微克/千克水平的水中和碱性土壤中三种磺酰脲类除草剂残留的方法。该方法基于固相萃取和带紫外检测的高效液相色谱法。在碱性土壤中,尤其是那些有机碳含量低的土壤,可以用去离子水提取除草剂,无需净化步骤。用工业级苯磺隆、甲磺隆和氯磺隆加标的土壤样品,通过与去离子水振荡1小时并以10,000转/分钟离心15分钟进行两次提取。通过玻璃微纤维滤器过滤的上清液以<20毫升/分钟的流速通过预先用甲醇和去离子水预处理过的C18柱。柱上保留的除草剂残留用酸化甲醇洗脱。洗脱液用高效液相色谱法分析。使用C18柱,流动相为甲醇/水(40 + 60,V/V),三种除草剂残留的检测限在水中和土壤中分别为1.0微克/升和3微克/千克。所研究的三种化合物的水样平均回收率为73 - 94%,而土壤样品的回收率为77 - 97%。

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