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 novel metal-organic framework (MOF) sorbent based on tannic acid/copper (TA/Cu) was synthesized and characterized for the application of the anticancer drug imatinib (IMA) from biological samples. The TA/Cu MOF was prepared via a facile coordination reaction and thoroughly characterized by SEM, XRD, and FTIR techniques. Critical parameters influencing the extraction efficiency of imatinib mesylate (IMAM), including pH, ionic strength, desorption solvent, and adsorption-desorption time were optimized. With acetonitrile as the desorption solvent, the method demonstrated a broad linear range of 0.55-300 μg L-1 under ideal conditions. Limits of detection and quantification were found to be 0.16 μg L-1 and 0.55 μg L-1, respectively.
... Show MoreA novel metal-organic framework (MOF) sorbent based on tannic acid/copper (TA/Cu) was synthesized and characterized for the application of the anticancer drug imatinib (IMA) from biological samples. The TA/Cu MOF was prepared via a facile coordination reaction and thoroughly characterized by SEM, XRD, and FTIR techniques. Critical parameters influencing the extraction efficiency of imatinib mesylate (IMAM), including pH, ionic strength, desorption solvent, and adsorption-desorption time were optimized. With acetonitrile as the desorption solvent, the method demonstrated a broad linear range of 0.55-300 μg L-1 under ideal conditions. Limits of detection and quantification were found to be 0.16 μg L-1 and 0.55 μg L-1, respectively.
... Show MoreTwo simple methods spectrophotometric were suggested for the determination of Cefixime (CFX) in pure form and pharmaceutical preparation. The first method is based without cloud point (CPE) on diazotization of the Cefixime drug by sodium nitrite at 5Cº followed by coupling with ortho nitro phenol in basic medium to form orange colour. The product was stabilized and measured 400 nm. Beer’s law was obeyed in the concentration range of (10-160) μg∙mL-1 Sandell’s sensitivity was 0.0888μg∙cm-1, the detection limit was 0.07896μg∙mL-1, and the limit of Quantitation was 0.085389μg∙mL-1.The second method was cloud point extraction (CPE) with using Trtion X-114 as surfactant. Beer
... Show MoreOrthogonal polynomials and their moments have significant role in image processing and computer vision field. One of the polynomials is discrete Hahn polynomials (DHaPs), which are used for compression, and feature extraction. However, when the moment order becomes high, they suffer from numerical instability. This paper proposes a fast approach for computing the high orders DHaPs. This work takes advantage of the multithread for the calculation of Hahn polynomials coefficients. To take advantage of the available processing capabilities, independent calculations are divided among threads. The research provides a distribution method to achieve a more balanced processing burden among the threads. The proposed methods are tested for va
... Show MoreThe new compounds of pyrazolines were synthesized from the reaction of different acid hydrazide with ethylacetoacetate and ethanol under reflux. These compounds were obtained from many sequence reactions. The 4-acetyl-5-methyl-2,4-dihydro-3H-pyrazol-3-one compounds synthesized from the reaction of 5-methyl-2,4-dihydro-3H-pyrazol-3-one with acetyl chloride in calcium hydroxide and 1,4-dioxane. Finaly, Schiff bases were prepared via condensation reaction of products of mono- and tri ketone derivatives[IV]a, b with phenyl hydrazines as presented in (Scheme 1, 2). The synthesized compounds were identification by using FTIR, NMR and Mass spectroscopy (of some of them).
Research Hypothesis from the fact that kicks off the effect that agricultural production in Iraq plays an important role in overcoming the food problem and achieving food security, but he became far far away from the provision of sufficient quantities of food products and then securing the Iraqi consumer food basket by the challenges faced by the agricultural sector.
To prove the hypothesis research in its structure in three axes came, the first axis eating historical significance to the subject of food over time periods as well as to clarify the concept of food security, and the second axis touched on the most important challenges facing the agricultural sector in Iraq and prevent the achievement of food requirements for members of
The adsorption study of thymol, was carried out at (25±0.1) °C, using granulated surfactant modified Iraqi Na – montmorillonite clay (initiated modified bentonite); in a down-flow packed column, the modified mineral was characterized by FT-IR spectroscopy. A linear calibration graph for thymol was obtained, which obey Beer's law in the concentration range of 5-50 mg/L at 274 nm against reagent blank. Single-factor-at-a-time approach; showed that the equilibrium time required for complete adsorption was 45 minute with flow rate (4.0drop/ mint). The adsorption of thymol increased with rising pH of the adsorbate solution, increase of solute uptake when the initial adsor
... Show MoreAll new compounds synthesized by many reactions starting from a product the compounds [I]a,b from reaction of 3-phenylenediamine or 4-phenylenediamine with chloroacetyl chloride, then the compounds [I]a,b reacted with potassium thiocyanate to yield compounds [II]a,b. While the compounds[III]a,b yield from reacted the compounds [I]a,b with sodium azide then the compounds [III]a,b reacted 1,3-dipolar cycloaddition reaction with acrylic acid to give compounds [IV]a,b and the later compounds reacted with phenylene diamine to product benzimidazole compounds [V]a,b . In addition to synthesized acid chloride compounds [VI]a,b by reacted the compounds [IV]a,b with thionyl chloride .Finally reacted the compounds [VI]a,b with different aromatic amine
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