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Optimization and Validation of a GC-FID/QuEChERS Method for Quantitative Determination of Spiromesifen Residues in Tomato Fruits, Leaves and Soil Matrices
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Pesticides serve a crucial function in contemporary farming practices, safeguarding agricultural crops against pest infestations and boosting production outputs. However, indiscriminate use has caused environmental and human health damage. This study aimed to develop and validate a gas chromatography-flame ionization detection (GC-FID) methodology for the direct and routine analysis of spiromesifen residues in soil, leaves, and tomato fruits. The proposed method prioritizes simplicity by avoiding derivatization steps, offering advantages over existing approaches that utilize lengthy multi-step extraction or derivatization prior to GC analysis. A key novelty of this work is the development of a QuEChERS extraction coupled directly to GC-FID without further clean-up or chemical treatment steps, rendering the method more convenient and accessible for routine monitoring applications. Factors evaluated included: sample solvent; inlet and column temperature profiles; inlet type; sample volume; and injection technique. Recovery and matrix effect studies were conducted by fortifying tomato, leaf, and soil matrices at three different concentrations (0.5, 1, and 10 µg ml-1). Quadruplicate analyses (n = 4) yielded mean recoveries of 98.74% (fruits), 93.92% (leaves), and 94.18% (soil), confirming efficient extraction. Matrix effects were negligible at -7.9%, -7.8%, and -5.3%, respectively. The chromatographic linearity of the developed GC-FID method was excellent over the 0.002–20 µg ml-1 range with R2 > 0.9979. The method demonstrated good precision, with inter- and intra-day RSD% ranging from 0.06–1.8%, below the 3% limit. GC-MS analysis confirmed spiromesifen identification. Under greenhouse conditions, residual levels were 1.39 mg/kg in soil, 8.24 mg/kg in tomato, and 3.39 mg/kg in leaves. Dissipation followed first-order kinetics with a half-life of 1.6 days. The optimized GC-FID method is promising for monitoring spiromesifen usage and guiding agricultural practices. © (2024), (Iranian Chemical Society). All rights reserved.

Scopus
Publication Date
Sun Mar 01 2015
Journal Name
Baghdad Science Journal
A New method for ISE construction for methyl orange dyes and using for indirect determination of Amitriptyline Hydrochloried drug
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A new method for construction ion-selective electrode (ISE) by heating reaction of methyl orange with ammonium reineckate using PVC as plasticizer for determination methyl orange and determination Amitriptyline Hydrochloried drug by formation ion-pair on electrode surface . The characteristics of the electrode and it response as following : internal solution 10-4M , pH (2.5-5) ,temperature (20-30) and response time 2 sec. Calibration response for methyl orange over the concentrationrange 10-3 -10-9 M with R=0.9989 , RSD%=0.1052, D.O.L=0.315X10-9 MEre%=(-0.877- -2.76) , Rec%.=(97.230 -101.711) .

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Publication Date
Tue Feb 01 2022
Journal Name
Baghdad Science Journal
Flow Injection Analysis with Turbidity Detection for the Quantitative Determination of Mebeverine Hydrochloride in Pharmaceutical Formulations
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The main objective of this paper is to develop and validate flow injection method, a precise, accurate, simple, economic, low cost and specific turbidimetric method for the quantitative determination of mebeverine hydrochloride (MbH) in pharmaceutical preparations.  A homemade NAG Dual & Solo (0-180º) analyser which contains two identical detections units (cell 1 and 2) was applied for turbidity measurements. The developed method was optimized for different chemical and physical parameters such as perception reagent concentrations, aqueous salts solutions, flow rate, the intensity of the sources light, sample volume, mixing coil and purge time. The correlation coefficients (r) of the developed method were 0.9980 and 0.9986 for cell

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Publication Date
Fri Feb 01 2019
Journal Name
Journal Of Economics And Administrative Sciences
Comparison of classical method and optimization methods for estimating parameters in nonlinear ordinary differential equation
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 ABSTRICT:

  This study is concerned with the estimation of constant  and time-varying parameters in non-linear ordinary differential equations, which do not have analytical solutions. The estimation is done in a multi-stage method where constant and time-varying parameters are estimated in a straight sequential way from several stages. In the first stage, the model of the differential equations is converted to a regression model that includes the state variables with their derivatives and then the estimation of the state variables and their derivatives in a penalized splines method and compensating the estimations in the regression model. In the second stage, the pseudo- least squares method was used to es

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Publication Date
Fri Jul 31 2020
Journal Name
Iraqi Geological Journal
APPLICATION OF TRIANGLES METHOD FOR QUANTITATIVE ESTIMATION OF MARL RESERVE IN EUPHRATES FORMATION, MIDDLE OF IRAQ
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Publication Date
Tue Aug 23 2016
Journal Name
International Journal Of Pharmacy And Pharmaceutical Sciences
QUALITATIVE PHYTOCHEMICAL COMPARISON BETWEEN FLAVONOIDS AND PHENOLIC ACIDS CONTENTS OF LEAVES AND FRUITS OF MELIA AZEDARACH (FAMILY: MELIACEAE) CULTIVATED IN IRAQ BY HPLC AND HPTLC
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<p><strong>Objective: </strong>The aim of our study was to compare between flavonoids and phenolic acids contents of leaves and fruits of <em>Melia azedarach</em> since no phytochemical investigation had done previously in Iraq.</p><p><strong>Methods: </strong>The leaves and fruits of <em>Melia azedarach </em>were extracted by soxhlet using 80% ethanol then the dried extract was suspended in water and fractionated using petroleum ether, chloroform, ethyl acetate, and n-butanol. The n-butanol fraction was hydrolyzed by acid and partitioned with ethyl acetate. The different fractions containing flavonoids and phenolic acids were analyzed by HPLC and HPTLC.</p><

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Publication Date
Mon Jul 21 2025
Journal Name
Journal Of Engineering
Correction Procedure for the Determination of Soil Specific Surface
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Publication Date
Wed Mar 15 2023
Journal Name
Journal Of Medicinal And Chemical Sciences
Simple Spectrophotometric Method for Determination of Drug Lisinopril in Pure Form and Pharmaceutical Formulations
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Scopus
Publication Date
Sat Jul 01 2023
Journal Name
Journal Of Analytical Chemistry
A Spectrophotometric Method for Tetracycline Determination in its Bulk Powder and Pharmaceutical Formulations Using Flow Injection and Batch Procedures: a Comparative Study
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A reliable and environmental analytical method was developed for the direct determination of tetracycline using flow injection analysis (FIA) and batch procedures with spectrophotometric detection. The developed method is based on the reaction between a chromogenic reagent (vanadium (III) solution) and tetracycline at room temperature and in a neutral medium, resulting in the formation of an intense brown product that shows maximum absorption at 395 nm. The analytical conditions were improved by the application of experimental design. The proposed method was successfully used to analyze samples of commercial medications and verified throughout the concentration ranges of 25–250 and 3–25 µg/mL for both FIA and batch procedures, respecti

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Publication Date
Mon Apr 28 2025
Journal Name
Chemical Papers
New chemiluminometric method for the determination of azithromycin in a continuous flow injection analysis system
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A novel analytical method is developed for the determination of azithromycin. The method utilizes continuous flow injection analysis to enhance the chemiluminescence system of luminol, H2O2, and Cr(III). The method demonstrated a linear dynamic range of 0.001–100 mmol L-1 with a high correlation coefficient (r) of 0.9978, and 0.001–150 mmol L-1 with a correlation coefficient (r) of 0.9769 for the chemiluminescence emission versus azithromycin concentration. The limit of detection (L.O.D.) of the method was found to be 18.725 ng.50 µL−1 based on the stepwise dilution method for the lowest concentration within the linear dynamic range of the calibration graph. The relative standard deviation (R.S.D. %) for n = 6 was less than 1.2%

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Publication Date
Sun Jun 03 2012
Journal Name
Baghdad Science Journal
Spectrofluorimetric method for the determination of glibenclamide in pharmaceutical formulations
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A sensitive spectrofluorimetric method for the determination of glibenclamide in its tablet formulations has been proposed. The method is based on the dissolving of glibenclamide in absolute ethanol and measuring the native fluorescence at 354 nm after excitation at 302 nm. Beers law is obeyed in the concentration of 1.4 to 10 µg.ml-1 of glibenclamide with a limit of detection (LD) of 0.067 µg.ml-1 and a standard deviation of 0.614. The range percent recoveries (N=3) is 94 - 103.

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