Simple and Rapid High-Performance Liquid Chromatography Method for Simultaneous Determination of Picloram and 2,4-D in Pesticide Formulations

Analytica Pub Date : 2022-11-20 DOI:10.3390/analytica3040029
A. Santilio, S. Girolimetti, V. Picardo
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Abstract

Picloram and 2,4-D are systemic herbicides used to control a wide range of broad-leaved weeds and post-emergence annual and perennial broad-leaved weeds, respectively. The use of plant protection products containing Picloram and 2,4-D necessitates the development of analytical methods, useful for the laboratories focused on control, for monitoring. In this study, we designed and validated an analytical method for the rapid determination of picloram and 2,4-D by HPLC-DAD. The method involves the extraction of the substances by sonication of the sample with methanol, followed by dilution in acetonitrile, and direct injection on a liquid chromatography system, based on the use of a Gemini C18 column. We used an isocratic mobile elution consisting of acetonitrile and water acidified 1% with H3PO4 (50:50, v/v). We validated the proposed method, which demonstrated linearity within the concentration range of 0.01–0.028 mg/mL for picloram and 2,4-D, with a correlation coefficient (R2) of 0.9993 for picloram and 0.9999 for 2,4-D. We considered precision, repeatability and selectivity in the validation. The repeatability of the method expressed as percent of relative standard deviation (%RSD) was lower than 1% for both substances. The proposed method is suitable for the simultaneous determination of picloram and 2,4-D in pesticide formulations.
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快速高效液相色谱法同时测定农药制剂中Picloram和2,4- d的含量
Picloram和2,4- d是一种系统除草剂,分别用于控制各种阔叶杂草和一年生和多年生阔叶杂草的萌发后。使用含有Picloram和2,4- d的植物保护产品,必须开发分析方法,以供侧重控制的实验室用于监测。本研究设计并验证了HPLC-DAD快速测定picloram和2,4- d的分析方法。该方法包括用甲醇对样品进行超声提取,然后在乙腈中稀释,然后在使用Gemini C18色谱柱的液相色谱系统上直接进样。我们使用了乙腈和1% H3PO4 (50:50, v/v)酸化的水组成的等密度流动洗脱液。结果表明,picloram和2,4- d在0.01 ~ 0.028 mg/mL的浓度范围内呈良好的线性关系,picloram和2,4- d的相关系数(R2)分别为0.9993和0.9999。我们在验证中考虑了精度、可重复性和选择性。该方法的重复性以相对标准偏差百分比(%RSD)表示,两种物质均低于1%。该方法适用于农药制剂中picloram和2,4- d的同时测定。
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