The development of a reversed phase high performance liquid chromatography fluorescence method for the determination of the mycotoxins fumonisin B1 and fumonisin B2 by using silica-based monolithic column is described. The samples were first extracted using acetonitrile:water (50:50, v/v) and purified by using a C18 solid phase extraction-based clean-up column. Then, pre-column derivatization for the analyte using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol was carried out. The developed method involved optimization of mobile phase composition using methanol and phosphate buffer, injection volume, temperature and flow rate. The liquid chromatographic separation was performed using a reversed phase Chromolith® RP-18e column (100 mm × 4.6 mm) at 30 °C and eluted with a mobile phase of a mixture of methanol and phosphate buffer pH 3.35 (78:22, v/v) at a flow rate of 1.0 mL min−1. The fumonisins separation was achieved in about 4 min, compared to approximately 20 min by using a C18 particle-packed column. The fluorescence excitation and emission were at 335 nm and 440 nm, respectively. The limits of detections were 0.01–0.04 μg g−1 fumonisin B1 and fumonisin B2, respectively. Good recoveries were found for spiked samples (0.1, 0.5, 1.5 μg g−1 fumonisins B1 and B2), ranging from 84.0 to 106.0% for fumonisin B1 and from 81.0 to 103.0% for fumonisin B2. Fifty-three samples were analyzed including 39 food and feeds and 14 inoculated corn and rice. Results show that 12.8% of the food and feed samples were contaminated with fumonisin B1 (range, 0.01–0.51 μg g−1) and fumonisin B2 (0.05 μg g−1). The total fumonisins in these samples however, do not exceed the legal limits established by the European Union of 0.8 μg g−1. Of the 14 inoculated samples, 57.1% contained fumonisin B1 (0.16–41.0 μg g−1) and fumonisin B2 (range, 0.22–50.0 μg g−1). Positive confirmation of selected samples was carried out using liquid chromatography–tandem mass spectrometry, using triple quadrupole analyzer and operated in the multiple reaction monitoring mode.
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.
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 spectrophotometric- reverse flow injection analysis (rFIA) method has been proposed for the determination of Nitrazepam (NIT) in pure and pharmaceutical preparations. The method is based upon the coupling reaction of NIT with a new reagent O-Coumaric acid (OCA) in the presence of sodium periodate in an aqueous solution. The blue color product was measured at 632 nm. The variation (chemical and physical parameters) related with reverse flow system were estimated. The linearity was over the range 15 - 450 µg/mL of NIT with detection limits and limit of quantification of 3.425 and 11.417 µg mL-1 NIT,respectively. The sample throughput of 28 samples
... Show MorePesticides 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
... Show MoreBackground: Mini implant stability is primarily related to local bone density; no studies have evaluated bone density related to mini implant placement for orthodontic anchorage between different age groups in the maxilla and the mandible. The present research aims to evaluate side, gender, age, and regional differences in bone density of the alveolar bone at various orthodontic implant sites. Materials and method: Fifty three individuals who were divided into two groups according to their age into: group I (ages 16-20 years) and group II (ages 21-29 years) had subjected to clinical examination, then 64-multislice computed tomography scan data were evaluated and bone density was measured in Hounsfield unit at 102 points (51 in the maxilla
... Show MoreIn this paper, a relationship between the liquid limit and the coefficient of consolidation of Iraqi soils are studied. The samples of soil used in study are undisturbed silty clay. These samples are taken from different locations and depths of Middle and South of Iraq by cooperation with Consulting Engineering Bureau- University of Baghdad- College of Engineering. The depth reached about 20 meters. The experimental work is made to calculate the liquid limit and the coefficient of consolidation. From these sites, 280 points are obtained. The relationship between the liquid limit and the coefficient of consolidation is drawn as a curve. This curve is studied and compared with the curve that obtained from other studies. From these curves, it
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions,
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected opti
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