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采用固相萃取结合气相色谱 - 氮磷检测器、气相色谱 - 质谱联用仪以及高效液相色谱 - 二极管阵列检测器对水中棉花脱叶剂、除草剂和杀虫剂残留进行多残留分析。

Multiresidue analysis of cotton defoliant, herbicide, and insecticide residues in water by solid-phase extraction and GC-NPD, GC-MS, and HPLC-diode array detection.

作者信息

Potter T L, Marti L, Belflower S, Truman C C

机构信息

USDA-ARS, Southeast Watershed Research Laboratory, P.O. Box 946, Tifton, Georgia 31793, USA.

出版信息

J Agric Food Chem. 2000 Sep;48(9):4103-8. doi: 10.1021/jf9909104.

DOI:10.1021/jf9909104
PMID:10995322
Abstract

A multiresidue procedure was developed for analysis of cotton pesticide and harvest-aid chemicals in water using solid-phase extraction and analysis by GC-NPD, GC-MS, and HPLC-DAD. Target compounds included the defoliants tribufos, dimethipin, thidiazuron; the herbicide diuron; and the insecticide methyl parathion. Three solid-phase extraction (SPE) media, octadecylsilyl (ODS), graphitized carbon black (GCB), and a divinylbenzene-N-vinyl pyrollidine copolymer (DVBVP), were evaluated. On GCB and ODS, recoveries varied depending on compound type. Recoveries were quantitative for all compounds on DVBVP, ranging from 87 to 115% in spiked deionized water and surface runoff. The method detection limit was less than 0.1 microg L(-)(1). SPE with DVBVP was applied to post-defoliation samples of surface runoff and tile drainage from a cotton research plot and surface runoff from a commercial field. The research plot was defoliated with a tank mixture of dimethipin and thidiazuron, and the commercial field, with tribufos. Dimethipin was detected (1.9-9.6 microg L(-)(1)) in all research plot samples. In the commercial field samples, tribufos concentration ranged from 0.1 to 135 microg L(-)(1). An exponentially decreasing concentration trend was observed with each successive storm event.

摘要

开发了一种多残留分析方法,用于分析水中的棉花农药和收获助剂化学品,该方法采用固相萃取,并通过气相色谱 - 氮磷检测器(GC-NPD)、气相色谱 - 质谱联用仪(GC-MS)和高效液相色谱 - 二极管阵列检测器(HPLC-DAD)进行分析。目标化合物包括脱叶剂三丁基膦、噻节因、噻苯隆;除草剂敌草隆;以及杀虫剂甲基对硫磷。评估了三种固相萃取(SPE)介质,即十八烷基硅烷(ODS)、石墨化炭黑(GCB)和二乙烯基苯 - N - 乙烯基吡咯烷共聚物(DVBVP)。在GCB和ODS上,回收率因化合物类型而异。在DVBVP上,所有化合物的回收率均为定量,在加标的去离子水和地表径流中的回收率范围为87%至115%。方法检测限小于0.1 μg L⁻¹。将DVBVP固相萃取应用于棉花研究地块的脱叶后地表径流和瓷砖排水样品以及商业田地的地表径流样品。研究地块用噻节因和噻苯隆的罐混液进行脱叶处理,商业田地用三丁基膦进行脱叶处理。在所有研究地块样品中均检测到噻节因(1.9 - 9.6 μg L⁻¹)。在商业田地样品中,三丁基膦浓度范围为0.1至135 μg L⁻¹。随着每次连续暴雨事件,观察到浓度呈指数下降趋势。

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