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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
Wed Mar 25 2015
Journal Name
Comptes Rendus Chimie
A novel method for the synthesis of biodiesel from soybean oil and urea
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The increasing demand for energy has encouraged the development of renewable resources and environmentally benign fuel such as biodiesel. In this study, ethyl fatty esters (EFEs), a major component of biodiesel fuel, were synthesized from soybean oil using sodium ethoxide as a catalyst. By-products were glycerol and difatty acyl urea (DFAU), which has biological characteristics, as antibiotics and antifungal medications. Both EFEs and DFAU have been characterized using Fourier transform infrared (FTIR) spectroscopy, and 1H nuclear magnetic resonance (NMR) technique. The optimum conditions were studied as a function of reaction time, reactant molar ratios, catalyst percentage and the effect of organic solvents. The conversion ratio of soybea

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Scopus
Publication Date
Sun Mar 02 2014
Journal Name
Baghdad Science Journal
With Solvent Extraction Method, and via new Organic Reagent 2-(Benzo thiazolyl azo)-4,5- Diphenyl Imidazole for Spectrophotometric Determination of Copper (II) in different Samples
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The new organic reagent 2-[Benzo thiazolyl azo]-4,5-diphenyl imidazole was prepared and used as complexing agent for separation and spectrophotometric determination of Cu2+ ion in some samples include plants, soil, water and human blood serum. Initially determined all factors effect on extraction method and the results show optimum pH was (pHex=9), optimum concentration was 40?g/5mLCu2+ and optimum shaking time was (15min.), as well stoichiometry study appears the complex structure was 1:1 Cu2+: BTADPI. Interferences effect of cations were studied. Synergism effect shows MIBK gave increasing in distribution ratio (D). Organic solvent effect appears there is no any linear relation between dielectric constant for organic solvent used and dis

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Publication Date
Sun Jun 02 2024
Journal Name
Methods And Objects Of Chemical Analysis
Simultaneous Spectrophotometric Determination of Piroxicam, Naproxen, Diclofenac Sodium and Mefenamic Acid in Pharmaceutical Formulations by Partial Least Squares Method
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A chemometric method, partial least squares regression (PLS) was applied for the simultaneous determination of piroxicam (PIR), naproxen (NAP), diclofenac sodium (DIC), and mefenamic acid (MEF) in synthetic mixtures and commercial formulations. The proposed method is based on the use of spectrophotometric data coupled with PLS multivariate calibration. The Spectra of drugs were recorded at concentrations in the linear range of 1.0 - 10 μg mL-1 for NAP and from 1.0 - 20 μg mL-1 for PIR, DIC, and MEF. 34 sets of mixtures were used for calibration and 10 sets of mixtures were used for validation in the wavelength range of 200 to 400 nm with the wavelength interval λ = 1 nm in methanol. This method has been used successfully to quant

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Publication Date
Wed Aug 01 2018
Journal Name
Journal Of Global Pharma Technology
GC/MS analysis of terpenes of Boswellia serrata resin found in Iraq
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Objective: The aim of this work was to detect terpenes other than boswellic acid derivatives in olibanum of Boswellia Serrata found in Iraq. Methods: The olibanum of Boswellia Serrata was macerated in methanol for one day, then filtration. Filter at was concentrated till reddish brown syrupy residue was gained, (3%) potassium hydroxide was added till basification. This basic solution was stirred continuously until a uniform emulsion was formed, then extracted with chloroform in a separatory funnel; the chloroform fraction was analyzed by GC /MS spectrometry. Results: GC /MS analysis reveal the presence of terpenes and non-terpenes constituents. Conclusion: Most of the detected terpenes were sesquiterpenes and the least one was di-terpenes.

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Scopus
Publication Date
Sun Jun 01 2014
Journal Name
Baghdad Science Journal
Spectrophotometric Analytical method for Determination the Drug Compound Salbutamol by using Prussian blue Complex
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This research aims to develop new spectrophotometric analytical method to determine drug compound Salbutamol by reaction it with ferric chloride in presence potassium ferricyanide in acid median to formation of Prussian blue complex to determine it by uv-vis spectrophotmetric at wavelengths rang(700-750)nm . Study the optimal experimental condition for determination drug and found the follows: 1- Volume of(10M) H2SO4 to determine of drug is 1.5 ml . 2- Volume and concentration of K3Fe(CN)6 is 1.5 ml ,0.2% . 3- Volume and concentration of FeCl3 is 2.5ml , 0.2%. 4- Temperature has been found 80 . 5- Reaction time is 15 minute . 6- Order of addition is (drug + K3Fe(CN)6+ FeCl3 + acid) . Concentration rang (0.025-5 ppm) , limit detecti

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Publication Date
Wed Apr 10 2013
Journal Name
Journal Of Materials Science And Engineering
Energy Transfer of Rhodamine110-Oxazine1 Mixtures Encapsulated in Glass Like Silica Xerogel Matrices
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Publication Date
Tue May 01 2018
Journal Name
Journal Of Physics: Conference Series
Performance of Case-Based Reasoning Retrieval Using Classification Based on Associations versus Jcolibri and FreeCBR: A Further Validation Study
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Publication Date
Mon Dec 01 2025
Journal Name
Journal Of Kufa For Chemical Sciences
A review on Chromatographic Techniques for the Determination of Pharmaceuticals in Environment
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The past several years have seen an increase in awareness of the pervasiveness of medications as pollutants in the aquatic environment. The main reason for concern regarding the release of pharmaceuticals into the environment is the possibility that biological agents may become opposing to them. The development of precise and reliable analytical techniques for pharmaceutical determination in a range of samples is necessary for their safe use in the pharmaceutical industry and medical treatments. This review offers a summary of chromatographic techniques for identifying and quantifying the examination of pharmaceuticals in a range of environmental samples. Both the general public and the scientific community are currently very intere

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Publication Date
Sun Sep 01 2024
Journal Name
Green Analytical Chemistry
Green methods for determination of paracetamol in drug samples: A comparative study
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Publication Date
Thu Feb 29 2024
Journal Name
Sabrao Journal Of Breeding And Genetics
LOW-‎COST SOIL ‎MOISTURE SENSORS’ ASSESSMENT FOR THEIR ACCURACY AFTER CALIBRATION THROUGH THE ‎GRAVIMETRIC METHOD
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The existing study aimed to assess four soil moisture sensors’ capacitive (WH51 and SKU: S EN0193) and resistive (Yl69 and IC Station) abilities, which are affordable and medium-priced for their accuracy in six common soil types in the central region of Iraq. The readings’ calibration for the soil moisture sensor devices continued through two gravimetric methods. The first depended on the protocols’ database, while the second was the traditional calibration method. The second method recorded the lowest analysis error compared with the first. The moderate-cost sensor WH51 showed the lowest standard error (SE), MAD , and RMSE and the highest R² in both methods. The performance accuracy of WH51 was close to readings shown by the manufac

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