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乙酰苯胺类除草剂降解产物的新型色谱分离及碳固相萃取

Novel chromatographic separation and carbon solid-phase extraction of acetanilide herbicide degradation products.

作者信息

Shoemaker Jody A

机构信息

U.S. Environmental Protection Agency, Office of Research and Development, National Exposure Research Laboratory, Cincinnati, OH 45268, USA.

出版信息

J AOAC Int. 2002 Nov-Dec;85(6):1331-7.

PMID:12477196
Abstract

One acetamide and 5 acetanilide herbicides are currently registered for use in the United States. Over the past several years, ethanesulfonic acid (ESA) and oxanilic acid (OA) degradation products of these acetanilide/acetamide herbicides have been found in U.S. ground waters and surface waters. Alachlor ESA and other acetanilide degradation products are listed on the U.S. Environmental Protection Agency's (EPA) 1998 Drinking Water Contaminant Candidate List. Consequently, EPA is interested in obtaining national occurrence data for these contaminants in drinking water. EPA currently does not have a method for determining these acetanilide degradation products in drinking water; therefore, a research method is being developed using liquid chromatography/negative ion electrospray/mass spectrometry with solid-phase extraction (SPE). A novel chromatographic separation of the acetochlor/alachlor ESA and OA structural isomers was developed which uses an ammonium acetate-methanol gradient combined with heating the analytical column to 70 degrees C. Twelve acetanilide degradates were extracted by SPE from 100 mL water samples using carbon cartridges with mean recoveries >90% and relative standard deviations < or =16%.

摘要

目前有1种乙酰胺类和5种乙酰苯胺类除草剂在美国登记使用。在过去几年中,在美国的地下水和地表水中发现了这些乙酰苯胺类/乙酰胺类除草剂的乙磺酸(ESA)和草氨酸(OA)降解产物。甲草胺ESA和其他乙酰苯胺类降解产物被列入美国环境保护局(EPA)1998年的饮用水污染物候选名单。因此,EPA有兴趣获取这些污染物在饮用水中的全国性出现数据。EPA目前没有测定饮用水中这些乙酰苯胺类降解产物的方法;因此,正在开发一种使用液相色谱/负离子电喷雾/质谱联用固相萃取(SPE)的研究方法。开发了一种新颖的色谱分离方法,用于分离乙草胺/甲草胺ESA和OA结构异构体,该方法使用醋酸铵 - 甲醇梯度,并将分析柱加热到70摄氏度。使用碳柱通过SPE从100 mL水样中萃取了12种乙酰苯胺类降解产物,平均回收率>90%,相对标准偏差<或 =16%。

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