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APPLICATION OF RAPID RESOLUTION LIQUID CHROMATOGRAPHY TO THE ANALYSIS OF SOME PESTICIDE RESIDUES IN APPLE JUICE
(Journal Agriculture and Forestry, 2017-09-30)
VELKOSKA-MARKOVSKA, Lenche
;
PETANOVSKA-ILIEVSKA, Biljana
;
MARKOVSKI, Aleksandar
This paper presents the application of a new, precise, accurate and reliable rapid resolution liquid chromatography (RRLC) method with ultraviolet-diode array detection (UV-DAD) for the determination of some organonitrogen and organophosphorus pesticide residues in apple juice samples. The successful separation and quantitative determination of analytes were achieved using a Poroshell EC 120-C18 (50 mm x 3 mm; 2.7 µm) analytical column maintained at 25 0C and the detection was monitored at 220 nm and 270 nm. The mixture of acetonitrile/water (50/50, V/V) was used as a mobile phase, with flow rate of 1 mL/min. Specificity, selectivity, linearity, precision, accuracy and limit of quantification (LOQ) were examined to assess the validity of the developed method according to European Commission guidelines for pesticide residue analytical methods and all the performance characteristics were found within acceptance criteria. The obtained values for multiple correlation coefficients (R2) were > 0.96, relative standard deviation (RSD) of retention times and peak areas were ≤ 1.15 %, and recoveries ranged from 93.98 % - 118.60 %, with RSD ≤ 1.77 %. The proposed method was successfully applied for the determination of investigated pesticides in apple juice samples. The detectable residues of examined pesticides were not found in the analysed samples.
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Application of High Performance Liquid Chromatography to the Analysis of Pesticide Residues in Apple Juice
(Walter de Gruyter GmbH, 2018-03-01)
Velkoska-Markovska, Lenche
;
Petanovska-Ilievska, Biljana
;
The modern apple production involves the use of large amounts of pesticides that can be found in processed products such as apple juice. Harmful effects of pesticide residues on humans, especially children, are well known, hence the content of pesticide residues in fruit, vegetables and their juices should be controlled. This study presents an application of a new, relatively simple and reliable analytical method for qualitative and quantitative determination of three organophosphorus and one organonitrogen pesticide residues in apple juices. The analysis utilizes reversed-phase high-performance liquid chromatography (RP-HPLC) followed by UV diode array detection. Prior to HPLC analysis, a solid-phase extraction (SPE) was used for analytes concentration and sample clean-up. Specificity, selectivity, linearity, precision, accuracy and limit of quantification (LOQ) were examined to assess the validity of the developed method. The method had satisfactory values of multiple correlation coefficients for calibration curves (R<jats:sup>2</jats:sup> ≥ 0.95 ). The precision was evaluated for the retention times and peak areas, and the estimated values for relative standard deviations (RSD) were 0.05 % - 0.18 % and 0.09 % - 0.62 %, respectively, which indicated an excellent precision of the proposed method. Under the established conditions, the recovery of analytes was 93.80 % - 119.41 %, with relative standard deviations below 0.56 %. This method was successfully applied for determination of some organophosphorus and organonitrogen pesticide residues in apple juices which were taken from Macedonian markets. The achieved values for LOQs were low enough compared to the MRLs of the investigated pesticides in apple according to the Regulation (EC) No 396/2005. Detectable residues of the examined pesticides were not found in the analyzed samples.</jats:p>

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