scholarly journals Application of High Performance Liquid Chromatography to the Analysis of Pesticide Residues in Apple Juice

2018 ◽  
Vol 67 (1) ◽  
pp. 93-102 ◽  
Author(s):  
Lenche Velkoska-Markovska ◽  
Biljana Petanovska-Ilievska ◽  
Aleksandar Markovski

Summary 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 (R2 ≥ 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.

2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.


2020 ◽  
Vol 17 (34) ◽  
pp. 1046-1054
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Saadiyah Ahmed DHAHIR

The triazole, tebuconazole pesticide, was determined in its formulation and also in the river water samples collected from different agriculture areas in the Iraqui city of Kerbala using developed high-performance liquid chromatography method(HPLC) with UV-visible detection, The mobile composition phase was a mixture of acetonitrile:methanol (50:50 v/v) and the column was C18 (250 cm x 4.6 mm,5μm). Also modified dispersive liquidliquid microextraction (DLLME), which is regarded as an ecological -friendly method, was used for the extraction of tebuconazole from water samples using acetonitrile and chloroform as solvents extraction and dispersive agent, respectively. Linearity to maintain the calibration curve was achieved from (0.1-70) μg.mL-1 with a limit of detection(0.053) μg.mL-1 and limit of quantification (0.174) μg.mL-1. Three spiked levels of concentration (1.0, 5.0, and 10) μg.mL-1 were used for the validation of the method. The relative standard deviation (RSD%) was (0.294- 0.813)%, and the percentage recovery was (100.001-100.005). The formulation studies for two different concentrations (10 and 40) μg.mL-1, which prepared from tebuconazole formulation (Raxil ODS2 2%), gave acceptable percentage recovery between (98.956-99.833). The developed method can be used accurately for the determination of tebuconazole in water samples and in the formulation of tebuconazole effectively.


2013 ◽  
Vol 781-784 ◽  
pp. 942-946 ◽  
Author(s):  
Jian Chao Deng ◽  
Xian Qing Yang ◽  
Lai Hao Li ◽  
Jian Wei Cen ◽  
Shu Xian Hao ◽  
...  

A new method of determination of malachite green (MG) in sediment has been developed by high performance liquid chromatography with fluorescence detection (HPLC-FLD). It is based on use of a deoxidation reaction which converts malachite green (MG) into LMG in the process of extraction. The sediment samples were extracted with a solution of formic acid and acetonitrile. Clean up and isolation was performed on MCX solid phase extraction (SPE) column. Chromatographic separation was achieved by using C18column with an isocratic mobile phase consisting of acetonitrile and ammonium acetate buffer (0.05 M, pH 4.5) (80:20, v/v). High performance liquid chromatography with fluorescence detector (λex=265 nm and λem=360 nm) was used for the determination of LMG. The recovery values of MG in sediment samples fortified with MG were determined by measuring the amount of MG in the samples, after carrying out deoxidation reaction with potassium borohydride, which converts the MG into LMG. Under the optimized conditions, the average recoveries of MG from sediment at three levels (1.0, 10 and 50 μg/kg) were 85.0% (range from 80.8 to 87.6%). Relative standard deviations (RSD) of recoveries at all fortification levels were less than for 9.57% for MG. The method detection limit obtained for MG was 0.5 μg/kg.


2006 ◽  
Vol 89 (2) ◽  
pp. 352-358 ◽  
Author(s):  
Jan Krzek ◽  
Jolanta Kaleta ◽  
Urszula Hubicka ◽  
Aneta Niedzwiedz

Abstract A reversed-phase high-performance liquid chromatography method with gradient elution was developed for the determination of the caffeic, p-coumaric, and ferulic acids in propolis concentrates. Solid-phase extraction on an RP18 column was applied for preliminary purification, and chromatographic separation was performed on 100 RP18e Lichrospher column of particle size 5 m. The mobile phase was obtained by mixing in appropriate ratios 0.03 mM NaH2PO4, acidified with H3PO4 up to pH 3.0, with acetonitrile to obtain a gradient in the elution process. Spectrophotometric detection was conducted at 320 nm. Under the established conditions, the method featured high sensitivity, good precision, and comparability of results, as proven by method validation and statistical analysis of the obtained results. The limits of detection were 0.315, 0.325, and 0.695 g/mL for caffeic, p-coumaric, and ferulic acids, respectively. The corresponding recovery values were 98.14, 101.05, and 99.42 and the linearity ranges from 1.31 to 99.18 g/mL, 1.52 to 119.16 g/mL, and 2.42 to 184.14 g/mL. The precision of the method was expresed by relative standard deviation values that did not exceed 3. It was also shown that the propolis concentrates under examination had similar antibacterial activity against Staphylococcus aureus ranging from 119.8 to 124.3 g/mL, contrary to model mixtures that showed no antibacterial activity.


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