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 MoreThree series of monomers, polymers and thioester cyclic compounds containing 4H-1,2,4-triazol-3-thiol moiety were synthesized and examined for their liquid crystalline properties. All monomers, polymers and thioester compounds were characterized by elemental analysis and FTIR, 1 H-NMR and mass spectroscopy. The phase transition and mesomorphic properties were investigated by polarized optical microscope (POM) and differential scanning calorimetry (DSC). The monomer with terminal phenyl substituent display dimorphism nematic and smectic A (SmA) mesophases. The corresponding polymers derived from acrylic and phenyl acrylic acid monomers show nematic mesophase. The only thioester cyclic compound derived from terephtaloyl chloride show nemati
... Show MoreCloud computing offers a new way of service provision by rearranging various resources over the Internet. The most important and popular cloud service is data storage. In order to preserve the privacy of data holders, data are often stored in cloud in an encrypted form. However, encrypted data introduce new challenges for cloud data deduplication, which becomes crucial for big data storage and processing in the cloud. Traditional deduplication schemes cannot work on encrypted data. Among these data, digital videos are fairly huge in terms of storage cost and size; and techniques that can help the legal aspects of video owner such as copyright protection and reducing the cloud storage cost and size are always desired. This paper focuses on v
... Show MoreThis research include synthesized and characterization the compound [I] by reaction terephthaldehyde , mercaptoacetic acid and thiosemicarbazide with concentrated sulfuric acid then this compound reaction with ethyl chloroacetate and sodium acetate to product ester compound [II],the latter compound reaction with hydrazine hydrate to synthesized acid hydrazide [III] after that reaction with 4-alkoxy benzaldehyde[IV]n to synthesized Schiff bases compounds [V]n, the compound [VI] synthesized via reaction compound [I] with chloroacetic acid and sodium acetate then the compound[VI] reaction with 2-phenylenediamine in 4 N hydrochloric acid to product benzimidazole compound[VII]. The compounds characterized by melting points, FTIR and 1HNMR spectr
... Show MoreThe new of compounds synthesized by sequence reactions starting from a reaction of 3-phenylenediamine or 4-phenylenediamine with chloroacetyl chloride to produce the compounds [I]a,b, then the compounds[I]a,b reacted with sodium azide to yield compounds[II]a,b that reacted 1,3-dipolarcycloaddition reaction with acrylic acid to give compounds [III]a,b these compounds reacted with methanol led to ester compounds[IV]a,b then reacted with hydrazine to give acid hydrazide [V]a,b . Finally compounds [V]a,b reacted with aromatic aldehydes to product shiff bases derivatives. The compounds characterized by mp. , IR, 1HNMR in addition to mass spectroscopy for some of them the liquid crystals properties were studied by using polarized optical microsco
... Show MoreThe research aims to derive the efficient industrial plans for Al – shaheed public company under risk by using Target MOTAD as a linear alternative model for the quadratic programming models.
The results showed that there had been a sort of (trade- off) between risk and the expected gross margins. And if the studied company strives to get high gross margin, it should tolerate risk and vice versa. So the management of Al- Shaheed Company to be invited to apply the suitable procedures in the production process, in order to get efficient plans that improves it's performance .
the study covered theoretical concering parial molal volume the applicability of jones-dole equation
Two 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 MoreThe research problem has crystallized and in light of these capabilities, the level of performance depends on the application of modern training methods based on actual experimentation, and those methods aim to develop the components of achievement in this competition, including the quantities of exerting the distinctive strength with speed for the arms and feet, which reflects on good skillful performance because the skill of shooting by jumping forward and high forms A major role in achieving goals during the competition that qualifies the team to win, and through the follow-up of the researcher in the field and academic field, I noticed that there is a weakness in some physical abilities, which affects performance and skill level
... Show MoreA newly developed analytical method was conducted for the determination of Ketotifen fumarate (KTF) in pharmaceuticals drugs via quenching of continuous fluorescence of 9(10H)-Acridone (ACD). The method was applied using flow injection system of a new homemade ISNAG fluorimeter with fluorescence measurements at ± 90◦ via 2×4 solar cell. The calibration graph was linear in the range of 1-45 mmol/L, with correlation coefficient r = 0.9762 and the limit of detection 29.785 µg/sample from the stepwise dilution for the minimum concentration in the linear dynamic ranged of the calibration graph. The method was successfully applied to the determination of Ketotifen fumarate in two different pharma
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