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.
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
... Show MoreA 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%
... Show MoreA 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.
A simple, rapid and sensitive spectrophotometric method has been developed for the determination of captopril in aqueous solution. The method is based on reaction of captopril with 2,3-dichloro 1,4- naphthoquinon(Dichlone) in neutral medium to form a stable yellow colored product which shows maximum absorption at 347 nm with molar absorptivity of 5.6 ×103 L.mole-1. cm-1. The proposed method is applied successfully for determination of captopril in commercial pharmaceutical tablets.
A UV-Vis spectrophotometry method was developed for the determination of metoclopramide hydrochloride in pure and several pharmaceutical preparations, such as Permosan tablets, Meclodin syrups, and Plasil ampoules. The method is based on the diazotization reaction of metoclopramide hydrochloride with sodium nitrate and hydrochloric acid to yield the diazonium salt, which is then reacted with 3,5-dimethyl phenol in the presence of sodium hydroxide to form a yellow azo dye. Calibration curves were linear in the range from 0.3 to 6.5 µg/mL, with a correlation coefficient of 0.9993. The limits of detection and quantification were determined and found to be 0.18 and 0.61 µg/mL, respectively. Accuracy and precision were also determined b
... Show MoreThe Cu(II) was found using a quick and uncomplicated procedure that involved reacting it with a freshly synthesized ligand to create an orange complex that had an absorbance peak of 481.5 nm in an acidic solution. The best conditions for the formation of the complex were studied from the concentration of the ligand, medium, the eff ect of the addition sequence, the eff ect of temperature, and the time of complex formation. The results obtained are scatter plot extending from 0.1–9 ppm and a linear range from 0.1–7 ppm. Relative standard deviation (RSD%) for n = 8 is less than 0.5, recovery % (R%) within acceptable values, correlation coeffi cient (r) equal 0.9986, coeffi cient of determination (r2) equal to 0.9973, and percentage capita
... Show Moreطريقة سهلة وبسيطة ودقيقة لتقدير السبروفلوكساسين في وجود السيفاليكسين او العكس بالعكس في خليط منهما. طبقت الطريقة المقترحة بطريقة الاضافة القياسية لنقطة بنجاح في تقدير السبروفلوكساسين بوجود السيفاليكسين كمتداخل عند الاطوال الموجية 240-272.3 نانوميتر وبتراكيز مختلفة من السبروفلوكساسين 4-18 مايكروغرام . مل-1 وكذلك تقدير السيفاليكسين بوجود السبروفلوكساسين الذي يتداخل باطوال موجية 262-285.7 نانوميتر وبتراكيز مخ
... Show MoreThis work reports the development of an analytical method for the simultaneous analysis of three fluoroquinolones; ciprofloxacin (CIP), norfloxacin (NOR) and ofloxacin (OFL) in soil matrix. The proposed method was performed by using microwave-assisted extraction (MAE), solid-phase extraction (SPE) for samples purification, and finally the pre-concentrated samples were analyzed by HPLC detector. In this study, various organic solvents were tested to extract the test compounds, and the extraction performance was evaluated by testing various parameters including extraction solvent, solvent volume, extraction time, temperature and number of the extraction cycles. The current method showed a good linearity over the concentration ranging from
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