Development and validation of a simple and efficient method for the analysis of commercial formulations containing clopyralid, picloram and aminopyralid as active ingredients.

Liquid chromatography plays a pivotal role in evaluating pesticide formulations as it enables the determination of multiple active substances in plant protection products. An adaptable separation technique has been developed, enabling the qualitative and quantitative analysis of clopyralid, picloram, and aminopyralid within pesticide formulations in line with SANCO/3030/99 rev. 5 guidelines. This article offers an insight into the validation procedure encompassing key aspects such as selectivity, linearity, accuracy, precision, and recovery. It places emphasis on critical stages, including sample preparation, chromatographic separation, detection, quantification, and data analysis. The active ingredients are separated using chromatography with isocratic elution, utilizing a mobile phase consisting of a mixture of water, acetonitrile, and acetic acid in a specific ratio (83:15:2 v/v/v). This separation is carried out on a YMC-Pack ODS-AQ column (250 mm x 4.6 mm, 5 µm) at a flow rate of 1.5 mL/min. The method's validation parameters have produced satisfactory outcomes. The recovery rates for each individual compound were found to be in the range of 98.6% to 101.0%. Precision, as indicated by the relative standard deviation (%RSD), was lower than the values predicted by the modified Horwitz equation. Furthermore, the correlation coefficients assessing the linearity of the response exceeded 0.99.

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

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-1 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-1 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.