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液相色谱法测定农药制剂中嘧菌酯及其杂质

Determination of azoxystrobin and its impurity in pesticide formulations by liquid chromatography.

作者信息

Marczewska Patrycja, Płonka Marlena, Rolnik Joanna, Sajewicz Mieczysław

机构信息

Pesticide Quality Testing Laboratory, Institute of Plant Protection - National Research Institute, Sosnicowice, Poland.

Department of General Chemistry and Chromatography, Institute of Chemistry, University of Silesia, Katowice, Poland.

出版信息

J Environ Sci Health B. 2020;55(7):599-603. doi: 10.1080/03601234.2020.1746572. Epub 2020 Apr 7.

DOI:10.1080/03601234.2020.1746572
PMID:32253976
Abstract

A method was developed for the simultaneous qualitative and quantitative determination of azoxystrobin and its relevant impurity (Z)-azoxystrobin using high performance liquid chromatography with diode array detector (HPLC-DAD) in suspension concentrate (SC) pesticide formulations, with the aim of the product quality control. Method validation was realized according to SANCO/3030/99 rev. 5. The proposed method was characterized by acceptable accuracy and precision. The repeatability expressed as ratio standard deviation (%RSD) to relative standard deviation (%RSDr) was lower than 1, whereas individual recoveries were in the range of 97-103% and 90-110% for azoxystrobin and (Z)-azoxystrobin, respectively. The limit of quantification (LOQ) for the impurity ((Z)-azoxystrobin) amounted to 0.3 µg mL and was acceptable because it was lower than the maximum permitted level according to Commission Implementing Regulation (EU) No 703/2011 of 20 July 2011 for the active substance (azoxystrobin) being 25 g kg of the azoxystrobin content found. The method described in this paper is simple, precise, accurate and selective as well as represents a new and reliable way of simultaneous determination of azoxystrobin and its relevant impurity in formulated products.

摘要

为实现悬浮剂(SC)农药制剂中嘧菌酯及其相关杂质(Z)-嘧菌酯的同时定性和定量测定,建立了一种采用二极管阵列检测器的高效液相色谱法(HPLC-DAD),目的是进行产品质量控制。方法验证按照SANCO/3030/99修订版5进行。所提出的方法具有可接受的准确度和精密度。以相对标准偏差(%RSD)与相对标准偏差(%RSDr)之比表示的重复性低于1,而嘧菌酯和(Z)-嘧菌酯的单个回收率分别在97-103%和90-110%范围内。杂质((Z)-嘧菌酯)的定量限(LOQ)为0.3μg/mL,这是可接受的,因为它低于2011年7月20日欧盟委员会实施条例(EU)No 703/2011中规定的活性物质(嘧菌酯)的最大允许水平,即嘧菌酯含量为25g/kg。本文所述方法简单、精确、准确且具有选择性,是一种同时测定制剂产品中嘧菌酯及其相关杂质的新的可靠方法。

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