A single step extraction-cleanup procedure using porous membrane-protected micro-solid phase extraction (μ-SPE) in conjunction with liquid chromatography–tandem mass spectrometry for the extraction and determination of aflatoxins (AFs) B1, B2, G1 and G2 from food was successfully developed. After the extraction, AFs were desorbed from the μ-SPE device by ultrasonication using acetonitrile. The optimum extraction conditions were: sorbent material, C8; sorbent mass, 20 mg; extraction time, 90 min; stirring speed, 1000 rpm; sample volume, 10 mL; desorption solvent, acetonitrile; solvent volume, 350 μL and ultrasonication period, 25 min without salt addition. Under the optimum conditions, enrichment factor of 11, 9, 9 and 10 for AFG2, AFG1, AFB2 and AFB1, respectively were achieved. Good linearity and correlation coefficient was obtained over the concentration range of 0.4–50 ng g−1 (r2 0.9988–0.9999 …
A rapid high performance liquid chromatography method for the determination of sphinganine (Sa) and sphingosine (So) in urine samples by employing a silica-based monolithic column is described. The samples were first extracted using ethyl acetate and derivatized using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol. C20 sphinganine was used as internal standard. Under the optimized conditions, separation was achieved using a mixture of methanol:water (93:7, v/v), column temperature at 30°C, flow rate of 1 mL min−1, and an injection volume of 10 μL. Good linearity was obtained for Sa and So over the concentration range 20–500 ng mL−1(correlation coefficients ≥0.9978). The detection limits were 0.45 ng mL−1 for Sa and
... Show MoreTwo simple, rapid, and useful spectrophotometric methods were suggest or the determination of sulphadimidine sodium (SDMS) with and without using cloud point extraction technique in pure form and pharmaceutical preparation. The first method was based on diazotization of the Sulphdimidine Sodium drug by sodium nitrite at 5 ºC, followed by coupling with α –Naphthol in basic medium to form an orange colored product . The product was stabilized and its absorption was measured at 473 nm. Beer’s law was obeyed in the concentration range of (1-12) μg∙ml-1. Sandell’s sensitivity was 0.03012 μg∙cm-1, the detection limit was 0.0277 μg∙ml-1, and the limit of Quantitation was 0.03605μg
... Show MoreThe current study investigated the stability and the extraction efficiency of emulsion liquid membrane (ELM) for Abamectin pesticide removal from aqueous solution. The stability was investigated in terms of droplet emulsion size distribution and emulsion breakage percent. The proposed ELM included a mixture of corn oil and kerosene (1:1) as a diluent, Span 80 (sorbitan monooleate) as a surfactant and hydrochloric acid (HCl) as a stripping agent without utilizing a carrier agent. Parameters such as homogenizer speed, surfactant concentration, emulsification time and internal to organic volume ratio (I/O) were evaluated. Results show that the lower droplet size of 0.9 µm and higher stable emulsion in terms of breakage percent of 1.12 % were
... Show MoreThe aim of this work was to develop and validate a rapid and low cost method for estimation of ibuprofen in pharmaceutical suspensions using Reverse-Phase High Performance Liquid Chromatography. The proposed method was conducted and validated according to International Conference on Harmonization (ICH) requirements. The chromatographic parameters were as follows: column of octyldecylsilyl C18 with dimensions (150 × 4.6) mm, mobile phase composed of acetonitrile with phosphoric acid with a ratio of 50 to 50 each using isocratic mode, flow rate of 1.5 mL/min and injection volume of 5 μL. The detection was carried out using UV detector at 220 nm. The method was validated and showed short retention time for ibuprofen peak at 7.651 min, wit
... Show MoreThe current study performed in order to detect and quantify epicatechin in two tea samples of Camellia sinensis (black and green tea) by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). Extraction of epicatechin from black and green tea was done by using two different methods: maceration (cold extraction method) and decoction (hot extraction method) involved using three different solvents which are absolute ethanol, 50% aqueous ethanol and water for both extraction methods using room temperature and direct heat respectively. Crude extracts of two tea samples that obtained from two methods were fractionated by using two solvents with different polarity (chloroform and
... Show MoreA simple and novel method was developed by combination of dispersive liquid-liquid microextraction with UV spectrophotometry for the preconcentartion and determination of trace amount of malathion. The presented method is based on using a small volume of ethylenechloride as the extraction solvent was dissolved in ethanol as the dispersive solvent, then the binary solution was rapidly injected by a syringe into the water sample containing malathion. The important parameters, such the type and volume of extraction solvent and disperser solvent, the effect of extraction time and rate, the effect of salt addition and reaction conditions were studied. At the optimum conditions, the calibration graph was linear in the range of 2-100 ng mL-1 of ma
... Show MoreAbsorption, fluorescence, quantum yield and lifetime of rhodamine 6G in chloroform, methanol and dimethyl sulfoxide were measured. From a comparison of these quantities, with those for solid solutions (solid solutions are obtained by mixing constant volume proportions of dye at a concentration of 1*10-4M/l with different volume proportions from the concentrated solution of polymer in chloroform and dimethyl sulfoxide). The results showed that the addition of polymer to liquid concentrated solutions (1*10-4M/l )of rhodamine 6G dye from expecting [which leading to development active medium for laser dye at high concentration] increase the spectra shift toward high energies, and the luminescence quantum yield but decreasing radiative lifetim
... Show MoreThe current study performed in order to detect and quantify epicatechin in two tea samples of Camellia sinensis (black and green tea) by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). Extraction of epicatechin from black and green tea was done by using two different methods: maceration (cold extraction method) and decoction (hot extraction method). Qualitative and quantitative determinations of epicatechin in two tea samples were investigated. Epicatechin identification was made by utilizing preliminary chemical tests and TLC. This identification was also boosted by HPLC and then quantified epicatechin in all ethyl acetate fractions of two tea samples. This research revealed the existence of epica
... Show MoreA simple, economical and selective method employing ion pair dispersive liquid−liquid microextraction (DLLME) coupled with spectrophotometric determination of carbamazepine (CBZ) in pharmaceutical preparations and biological samples was developed. The method is based on reduction of Mo(VI) to Mo(V) using a combination of ammonium thiocyanate and ascorbic acid in acidic medium to form a red binary Mo(V) thiocyanate complex. After addition of CBZ to the complex, extraction of the formed CBZ−Mo(V)−(SCN)6 was performed using a mixture of methylene chloride and methanol. Then, the measurement of target complex was performed at the wavelength of 470 nm. The important extraction parameters affecting the efficiency of DLLME were studied and o
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