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 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 MoreA 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.
This 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
... 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 MoreThis paper present a simple and sensitive method for the determination of DL-Histidine using FIA-Chemiluminometric measurement resulted from oxidation of luminol molecule by hydrogen peroxide in alkaline medium in the presence of DL-Histidine. Using 70?l. sample linear plot with a coefficient of determination 95.79% for (5-60) mmol.L-1 while for a quadratic relation C.O.D = 96.44% for (5-80) mmol.L-1 and found that guadratic plot in more representative. Limit of detection was 31.93 ?g DL-Histidine (S/N = 3), repeatability of measurement was less that 5% (n=6). Positive and negative ion interferances was removed by using minicolume containing ion exchange resin located after injection valve position.
Two simple and sensitive spectrophotometric methods are proposed for the determination of amitriptyline in its pure form and in tablets. The first method is based on the formation of charge- transfer complex between amitriptyline as n-donor and tetracyano-ethylene (TCNE) as πacceptor. The product exhibit absorbance maximum at 470 nm in acetonitrile solvent (pH =9.0 ) . In the second method the absorbance of the ion- pair complex, which is formed between the soughted drug and bromocresol green (BCG), was measured at 415 nm at ( pH=3.5) . In addition to classical univariate optimization, modified simplex method (MSM) was applied in the optimization of the variable affecting the color producing reaction by a geometric simple
... Show MoreTwo different approaches, univariate and multivariate (simplex method), have been used to obtain the optimum conditions for the quantitative Spectrophotometric determination of Eu3+ using Solochrome violet RS (3-Hydroxy-4-(2-hydroxy phenyl azo) naphthalene -1sulfonic acid) (SVRS) as a chromogenic reagent. The investigation shows that Eu3+ ion forms a wine-red complex with SVRS in alkaline buffer solution having a maximum absorbance at 464 nm against reagent blank. Calibration graphs obtained under univariate and simplex were found to be linear in the range of (0.30-8.0) µg/ml with detection limit 0.061µg/ml and molar absorptivity of 9877.66 L/mol.cm and (0.40-10.0)µg/ml with
... Show MoreCharge transfer complex formation method has been applied for the spectrophotometric determination of cimetidine, in bulk sample and dosage form. The method was accurate, simple, rapid, inexpensive and sensitive depending on the formed charge- transfer complex between cited drug and, 2,3-Dichloro-5,6-dicyano-p- benzoquinone (DDQ) as a chromogenic reagent. The formed complex shows absorbance maxima at 587 nm against reagent blank. The calibration graph is linear in the ranges of (5.0 - 50.0) µg.mL-1 with detection limit of 0.268µg.mL-1. The results show the absence of interferences from the excipients on the determination of the drug. Therefore the proposed method has been successfully applied for the determination of cimetid
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