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Rapid resolution liquid chromatography method for determination of malathion in pesticide formulation

Velkoska-Markovska L., Petanovska-Ilievska B.

Acta Chromatographica

2020

Vol. 32, no. 4

256--259

This paper presents a new, simple, precise, and accurate rapid resolution liquid chromatography (RRLC) method for determination of an active ingredient malathion in the pesticide formulation. The analysis was performed on a Poroshell EC 120-C18 (50 mm × 3 mm, 2.7 μm) analytical column using isocratic elution with a mobile phase consisted of acetonitrile–water (50:50, v/v), a flow rate of 1 mL/min, a constant column temperature at 25 °C, and ultraviolet-diode array detection (UV-DAD) at 220 nm. The specificity, selectivity, linearity, precision, and accuracy were tested for the method validation according to the Collaborative International Pesticides Analytical Council (CIPAC) and Directorate General Health and Consumer Protection (SANCO) guidelines and all tested parameters were found within acceptance criteria. The obtained results indicated that the proposed method can be used for routine analysis of the active ingredient malathion in the pesticide formulation “Etiol tecni” following the CIPAC and SANCO rules. The run time of analysis under the stipulated chromatographic conditions was about 2.5 min, meaning that the proposed method requires a small volume (< 1.5 mL) of the organic solvent (acetonitrile) making it cost-effective.

Development and validation of high-performance liquid chromatography method for determination of some pesticide residues in table grape

Velkoska-Markovska L., Petanovska-Ilievska B., Jankulovska M. S., Ilievski U.

Acta Chromatographica

2018

Vol. 30, no. 4

250--254

This study presents the development and validation of a new reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous determination of captan, folpet, and metalaxyl residues in table grape samples with ultraviolet–diode array detection (UV–DAD). Successful separation and quantitative determination of analytes was carried out on LiChrospher 60 RP-select B (250 × 4 mm, 5 μm) analytical column. Mixture of acetonitrile–0.1% formic acid in water (65:35, v/v) was used as a mobile phase, with flow rate of 1 mL/min, constant column temperature at 25 °C, and UV detection at 220 nm. The target residues were extracted with acetone by ultrasonication, followed by a cleanup using liquid–liquid extraction (LLE) and solid-phase extraction (SPE). The obtained values for multiple correlation coefficients (R2 > 0.90), relative standard deviation (RSD) of retention times, peak areas and heights (RSD ≤ 2.25%), and recoveries ranging from 90.55% to 105.40%, with RSD of 0.02% to 5.37%, revealed that the developed method has a good linearity, precision, and accuracy for all analytes. Hence, it is suitable for routine determination of investigated fungicides in table grape samples.