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.
Organohalosilanes conslitute an important subject ١٦؛ the chemistry oforganosilicon compound؛. Being starting materials and intermediates in the synthesis of a large number of various compounds so it is very important to get such materials in its highest purity ,but the separation of rathylchlorosilanes was still a big^oblem, duet^the great similarity in their physical and chemical properties, making its analysing verydifficult, ^or this reason tteir must be a good method o^e^r^iondealing^ththe^compounds, gas- liquid chromatography proved that it was the best, specially when (m- nitrotoluene) was used as a stationary liquid phase, it gave a complete separation and a good statistical results
The solvent free oxidation of benzyl alcohol was conducted employing Au and Pd supported catalysts, while utilizing hydrogen peroxide 35% (H2O2) as the oxidant, H2O2 is very cheap, mild, and an environment friendly reagent, which produced water as the only by-product. Various proportions of Au-Pd catalysts on carbon and titanium oxide activated as supports were synthesized through the use of sol immobilization catalyst synthesis technique. Characterization of the synthesized catalysts was performed using X-Ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), Field Emission Scanning Electron Microscopy (FESEM), and Transmission Electron Microscopy (TEM). It was found that the synthesized Au-Pd/ activated carbon catalyst was benef
... Show MoreThe present work establishes and validates HILIC strategies simple, accurate, exact and precise in pure form and inpharmaceutical dosage for separating and determining theophylline. These methods are developed on HILIC theophyllineseparation in columns ZIC2 and ZIC3. The eluent was prepared by mixing buffer (20% sodium acetate-40 mM, pH 5.5), 80%acetonitrile. The flow rate is 0.8 mL/min, with gradient elution and UV detection at 270 nm. In the ZIC2 and ZIC3 columns oftheophylline determining, the concentration range was 0.01-4μg.ml-1. The lower limit of detection and quantification fortheophylline were determined as 0.130, 0.190 μg.ml-1 and accuracy were 99.70%, 99.58% on ZIC2 and ZIC3, respectively. TheHILIC methods developed and validat
... Show MoreThis research adopts the estimation of mass transfer coefficient in batch packed bed distillation column as function of physical properties, liquid to vapour molar rates ratio (L / V), relative volatility (α), ratio of vapour and liquid diffusivities (DV / DL), ratio of vapour and liquid densities (ρV / ρL), ratio of vapour and liquid viscosities (μV/ μL).
The experiments are done using binary systems, (Ethanol Water), (Methanol Water), (Methanol Ethanol), (Benzene Hexane), (Benzene Toluene). Statistical program (multiple regression analysis) is used for estimating the overall mass transfer coefficient of vapour and liquid phases (KOV and KOL) in a correlation which represented the data fairly well.
KOV = 3.3 * 10-10
... Show MoreTwo simple methods for the determination of eugenol were developed. The first depends on the oxidative coupling of eugenol with p-amino-N,N-dimethylaniline (PADA) in the presence of K3[Fe(CN)6]. A linear regression calibration plot for eugenol was constructed at 600 nm, within a concentration range of 0.25-2.50 μg.mL–1 and a correlation coefficient (r) value of 0.9988. The limits of detection (LOD) and quantitation (LOQ) were 0.086 and 0.284 μg.mL–1, respectively. The second method is based on the dispersive liquid-liquid microextraction of the derivatized oxidative coupling product of eugenol with PADA. Under the optimized extraction procedure, the extracted colored product was determined spectrophotometrically at 618 nm. A l
... Show MoreLiquefied petroleum gases (LPG) consist of hydrocarbons obtained by refining crude oil, either from propane or butane or a mixture of the two. There are often other components such as propylene, butylene or other hydrocarbons, but they are not the main component. The study aims to review previous studies dealing with designing an LPG system to deliver gas to residential campuses and buildings. LPG is extracted from natural gas NG by several processes, passing through fractionation towers and then pressuring into CNG storage tanks. Gas contains several problems, including gas leakage through the pipes and leads to fires or explosions in LPG storage and distribution tanks, so safety conditions were taken in the design and implementation. T
... 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 investigation is a study of the length of time where drops can exist at an oil-water interface before coalescence take place with a bulk of the same phase as the drops. Many factors affecting the time of coalescence were studied in is investigation which included: dispersed phase flow rate, continuous phase height, hole size in distributor, density difference between phases, and viscosity ratio of oil/water systems, employing three liquid/liquid systems; kerosene/water, gasoil/water, and hexane/water. Higher value of coalescence time was 8.26 s at 0.7ml/ s flow rate, 30cm height and 7mm diameter of hole for gas oil/water system, and lower value was 0.5s at 0.3ml/s flow rate, 10 cm height and 3mm diameter of hole for hexane
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