Omid Reza Heravizadeh, Monireh Khadem, Ramin Nabizadeh, Seyed Jamaleddin Shahtaheri,
Volume 9, Issue 3 (9-2019)
Abstract
Introduction: Along with the extensive production and use of various pesticides for controlling pests and enhancing the production of agricultural crops, there is a growing concern about the adverse effects of these toxic materials on human health. Therefore, the development of sensitive, selective, and accurate methods for continuous assessment of pesticides concentration in occupational and environmental fields and comparing them with national and international standards is of great importance. This study was aimed at synthesis and application of molecularly imprinted polymer as a selective sorbent for residue determination of two pyrethroid isomers in biological samples.
Material and Methods: The MIP particles were prepared by a non-covalent approach using permethrin as a template, chloroform as progen solvent, methacrylic acid as functional monomer and ethyleneglycol dimethacrylate as cross-linker, at 55 °C for 18 hours in an oil bath. Field emission scanning electron microscopy was used to investigate the morphology and size of polymer particles. Afterward, the critical parameters, which could affect the recognition properties of synthesized MIP, were investigated and optimized under the selected operational ranges for the highest adsorption and recycling yield in solid-phase extraction of permethrin in biological samples
Results: using precipitation polymerization technique, uniform and spherical particles with the nano-ranged diameter (less than 21.2 nanometers) were obtained. Under the optimized condition, the designed molecularly imprinted solid-phase extraction (MISPE) technique exhibited great potential for the extraction of pesticide isomers in the real sample. More than 93 % of the recovery obtained from spiked urine samples. The linear calibration curve was obtained from 20-120 μg.L-1 (R2=0.99) and the detection limit was less than 6 ppb for both isomers. The presence of interferences had no effect on the selectivity of the method up to 100-fold.
Conclusion: employing the molecular imprinted solid-phase extraction method along with the high-performance liquid chromatography technique resulted in a selective and sensitive approach, suitable for quantitative monitoring of the desired pesticide in complex biological samples.
Somayeh Kamgou, Khosrou Abdi, Monire Khadem, Mahmoud Heidari, Omid Heravizadeh, Ali Daneyali, Seyed Jamaloddin Shahtaheri,
Volume 10, Issue 1 (3-2020)
Abstract
Introduction: Todays, exposure to heavy metals is happened by being produced in various environmental, industrial processes. The production of metals finally results in air pollution as well as contamination in the food chain. There are harmful effects of heavy metals such as cadmium on different organs. Therefore, this study aimed to identify and quantify cadmium in biological samples using DLLME SFOD method.
Materials and Methods: Optimization of the underlying variables played a key role in the process including sample PH, chelator, extractor and disperser solvents, ion concentration, time and rate of centrifugation and extraction time. It was done by employing central composite design (CCD) of the response surface methodology. In the process of optimization, after setting a certain pH, Specific salt concentration and ditizon added to form a complex between the metal and the chelator. A mixture of extraction and dispersant solvents added to the sample. The organic and aqueous phase separations when centrifugation and vortex carried out, the sample vial transferred to a cold ice bath and the organic solvent floated on the aqueous solvent .The organic portion containing the analyte was injected into the analyzer apparatus.
Results. The results showed that variables such as sample PH, complexing solvent, extraction solvent, centrifugation effect and extraction time play an important role in the extraction of cadmium metal ion from biological samples. The optimized method with a minimum detection limit (LOD) of 2 μg / l and a concentration factor (EF) of 50 and a relative recovery (RR) of 1.06.26 used to extract cadmium from urine samples.
Conclusion. According to the pre-test results and the optimization process, they showed that in the three factors of sample PH, salt concentration and extraction solvent volume that play a more effective role in cadmium extraction by DLLME-SFOD method.
