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

• Published in: Journal of environmental science and health. Part B, Pesticides, food contaminants, and agricultural wastes Vol. 59; no. 5; pp. 209 - 214
• Main Authors: Marczewska, Patrycja, Rolnik, Joanna, Szalbot, Monika, Stobiecki, Tomasz
• Format: Journal Article
• Language: English
• Published: England Taylor & Francis 2024; Taylor & Francis Ltd
• Subjects: Acetic acid; Acetonitrile; Active substance; Chromatography; Correlation coefficient; Correlation coefficients; Data analysis; Flow rates; Formulations; HPLC; Ingredients; Linearity; Liquid chromatography; nonselective signals; pesticide formulations; Pesticides; Picloram; Plant protection; Qualitative analysis; quality of plant protection products; Recovery; Sample preparation; Separation; quality of plant protection products; nonselective signals; Active substance; HPLC; pesticide formulations
• ISSN: 0360-1234; 1532-4109
• DOI: 10.1080/03601234.2024.2323425

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.