Maryam Ramin Sabet, Mehran Pourhossein, Monireh Khadem, Fariborz Omidi, Farideh Golbabaei, Seyed Jamaleddin Shahtaheri,
Volume 8, Issue 4 (12-2018)
Abstract
Introduction: Measurement of pesticides in biological matrices is become a serious challenge for researchers due to their very low concentration in different matrices. The aim of this study was to develop a new sample preparation method with high accuracy and validity and short retention time for determination of diazinon.
Material and Method: Dispersive liquid-liquid micro-extraction technique coupled with high performance liquid chromatography equipped with ultra violet detector was developed for trace extraction and determination of diazinon pesticide in human urine samples. One variable at a time method was used to optimize parameters affecting the diazinon extraction. Different parameters such as extraction solvent, disperser solvent, and volume of the extraction solvent, volume of the disperser solvent, centrifugation time and speed, salt addition, and sample pH were studied and optimized.
Result: Findings showed that optimal levels of these variables for diazinon pesticide were 150 μl of carbon tetrachloride as extraction solvent, 1.5 ml of methanol as dispersive solvent, pH of 6, 5 minutes centrifuge time at speed of 4000 rpm , 0% (w/v) salt addition. Correlation coefficient was 0.9965 indicating the linearity of a wide range of concentrations of the toxin. LOD and LOQ was calculated less than 0.7 and 5 µg L-1 respectively. The relative standard deviation for six replicate experiments in intra-day and inter-day at tree selected concentrations (50, 200 and 1000 µg L-1) was less than 4% that indicates the accuracy and precision of the optimized method. Enrichment factor and extraction recovery for diazinon were 245 and 99% respectively.
Conclusion: According to the results, dispersive liquid-liquid micro-extraction procedure was successfully developed for the extraction of diazinon from human urine samples. Compared to other extraction techniques, the proposed procedure had some advantages such as shorter extraction time, better reproducibility, and higher enrichment factor.
Nematullah Kurd, Abdulrahman Bahrami, Abbas Afkhami, Farshid Ghorbani Shahna, Mohammad Javad Assari, Maryam Farhadian,
Volume 13, Issue 3 (9-2023)
Abstract
Introduction: Toluene, benzene, xylene, and ethylbenzene (BTEX) belong to the class of monocyclic aromatic hydrocarbons and are identified as toxic volatile compounds due to their harmful properties. The reliable biomarkers for occupational exposure to these toxic compounds are hippuric acid (HA), trans,trans-muconic acid (tt-MA), mandelic acid (MA), and methylhippuric acid (MHA), which correlate with toluene, benzene, ethylbenzene, and xylene, respectively.
Material and Methods: A novel magnetized imine-linked covalent organic framework (Fe3O4@TFPA-Bd) was synthesized, marking its inaugural use as a sorbent in microextraction by packed sorbent (MEPS). The synthesis of Fe3O4@TFPA-Bd was executed in a straightforward and efficient manner, using Fe3O4 nanoparticles as the magnetic core and benzidine (Bd) and Tris (4-formyl phenyl) amine (TFPA) as the structural building blocks. This newly produced sorbent was tested for the microextraction of hippuric acid (HA), mandelic acid (MA), trans, trans-muconic acid (tt-MA), and m-methyl hippuric acid (m-MHA) from urine samples, which were then analyzed using high-performance liquid chromatography (HPLC). In order to optimize the extraction performance, parameters like sample volume, elution volume, extraction cycles, pH, and sample solution temperature were thoroughly adjusted. The synthesized adsorbent underwent thorough characterization via scanning and transmission electron microscopy (SEM and TEM), Fourier transforms infrared spectrometer (FTIR), and X-ray diffraction (XRD).
Results: The developed method showcased promising attributes: low detection limits (0.02 µg/ml for tt-MA, S/N=3), low quantification limits (0.06 µg/ml for tt-MA, S/N=10), a solid linear range (0.5-320 µg/ml for MA, R > 0.99), and commendable intra- and inter-day precision (2.4%-4.3% and 3.1%-7.8%, respectively) for volatile organic compound (VOC) biomarkers. Furthermore, the method demonstrated recoveries in the 81-87.5% range for spiked samples, indicating its practicality and effectiveness.
Conclusion: The developed procedure was suitable for the determination of BTEX biomarkers from urine samples and can be an alternative to previous methods.
