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高效液相色谱法(HPLC)作为监测氟唑菌酰胺在土壤中命运的工具。

High-performance liquid chromatography (HPLC) as a tool for monitoring the fate of fluazinam in soil.

机构信息

a Department of Food and Environmental Sciences , University of Helsinki , Helsinki , Finland.

出版信息

J Environ Sci Health B. 2014;49(7):491-7. doi: 10.1080/03601234.2014.896669.

DOI:10.1080/03601234.2014.896669
PMID:24813983
Abstract

Fluazinam is a widely used pesticide employed against the fungal disease late blight in potato cultivation. A specific, repeatable, and rapid high-performance liquid chromatography (HPLC) method utilizing a diode array detector (DAD) was developed to determine the presence of fluazinam in soil. The method consists of acetonitrile (ACN) extraction, clean-up with solid-phase extraction (SPE), and separation using a mobile phase consisting of 70% ACN and 30% water (v/v), including 0.02% acetic acid. HPLC was performed with a C18 column and the detection wavelength was 240 nm. The method was successfully applied to an incubation experiment and to soil samples taken from potato fields where fluazinam had been applied two to three times during the on-going growing season. In the 90-day incubation experiment, analytical standard fluazinam and the commercial fungicide Shirlan(®) were added to soil samples that had never been treated with fluazinam, and were then extracted with ACN and 0.01 M calcium chloride (CaCl2). Fluazinam was not extractable with CaCl2, indicating that it does not leach to watercourses in the dissolved form. Recovery with ACN extraction for sandy soils was 72-95% immediately after application and 53-73% after 90 days of incubation. Out of the eight potato field soil samples, fluazinam was found in two samples at concentrations of 2.1 mg kg(-1) and 1.9 mg kg(-1), well above the limit of quantification (0.1 mg kg(-1)).

摘要

氟唑菌酰胺是一种广泛应用于防治马铃薯晚疫病的农药。本研究建立了一种利用二极管阵列检测器(DAD)的特定、可重复、快速的高效液相色谱(HPLC)方法,用于检测土壤中氟唑菌酰胺的残留。该方法采用乙腈(ACN)提取,固相萃取(SPE)净化,流动相为 70% ACN 和 30%水(v/v),其中含有 0.02%乙酸。采用 C18 柱进行 HPLC 分析,检测波长为 240nm。该方法成功应用于一项为期 90 天的孵化实验以及从正在生长季节中已使用氟唑菌酰胺 2-3 次的马铃薯田采集的土壤样品中。在 90 天的孵化实验中,分析标准氟唑菌酰胺和商业杀菌剂 Shirlan(®)被添加到从未用过氟唑菌酰胺的土壤样品中,然后用乙腈和 0.01 M 氯化钙(CaCl2)提取。氟唑菌酰胺不能用 CaCl2 提取,表明其不会以溶解形式淋滤到水道中。立即施药后,沙土中用 ACN 提取的回收率为 72-95%,90 天后的回收率为 53-73%。在 8 个马铃薯田土壤样品中,有两个样品中检测到氟唑菌酰胺,浓度分别为 2.1mgkg(-1)和 1.9mgkg(-1),远高于定量限(0.1mgkg(-1))。

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