A 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 optimized in detail. At the optimum conditions, the linear range was 0.02–0.2 µg/mL. Moreover, the limits of detection and quantification were 0.01 and 0.04 µg/mL, respectively. High enrichment factor was obtained (118). Good recoveries at 0.06, 0.15 and 0.2 µg/mL ranging from 93 to 102% were achieved. The proposed method was successfully applied to the determination of CBZ in pharmaceutical formulations and biological samples.
Simple, precise and economic batch and flow injection analysis (FIA)-spectrophotometric methods have been established for simultaneous determination of salbutamol sulfate (SLB) in bulk powder and pharmaceutical forms. Both methods based on diazotization coupling reaction of SLB with another drug compound (sulfadimidine) as a safe and green diazotization agent in alkaline medium. At 444 nm, the maximum absorption of the orange azo-dye product was observed. A thorough investigation of all chemical and physical factors was conducted for batch and FIA procedures to achieve high sensitivity. Under the optimized experimental variables, SLB obeys Beer’s law in the concentration range of 0.25-4 and 10-100 μg/mL with limits of detection o
... Show MoreA simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations
... Show MoreLiquid electrodes of domperidone maleate (DOMP) imprinted polymer were synthesis based on precipitation polymerization mechanism. The molecularly imprinted (MIP) and non-imprinted (NIP) polymers were synthesized using DOMP as a template. By methyl methacrylate (MMA) as monomer, N,Nmethylenebisacrylamide (NMAA) and ethylene glycol dimethacrylate (EGDMA) as cross-linkers and benzoyl peroxide (BP) as an initiator. The molecularly imprinted membranes were synthesis using acetophenone (APH), di-butyl sabacate (DBS), Di octylphthalate (DOPH) and triolyl phosphate (TP)as plasticizers in PVC matrix. The slopes and limit of detection of l
... Show MoreA new colorimetric-flow injection method has been developed and validated for the detection of Cefotaxime sodium in pharmaceutical formulations. This method stands out for its rapid and sensitive nature. The formation of a brown-colored complex between Cefotaxime sodium and the Biuret reagent in a highly alkaline environment serves as the basis for the detection. The intensity of this colored complex is measured using a custom-built Continuous Flow Injection Analyzer, enabling accurate quantification of Cefotaxime sodium. Optimization studies of the chemical and physical parameters such as dilution of Biuret reagent, effect of the medium basicity, flow rate, sample loop and others have been investigated. The calibration gra
... 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
... Show MoreIn this paper, turbidimetric and reversed-phase ultra-fast liquid chromatography (UFLC) methods were described for the quantitative determination of ephedrine hydrochloride in pharmaceutical injections form. The first method is based on measuring the turbidimetric values for the formed yellowish white precipitate in suspension status in order to determine the ephedrine hydrochloride concentration. The suspended substance is formed as a result of the reaction of ephedrine hydrochloride with phosphomolybdic acid which was used as a reagent. The physical and chemical characteristics of the complex were investigated. The calibration graphs of ephedrine were established by turbidity method. While the second method (UFLC) was conducted using the
... Show MoreA 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
... Show MoreIn this study, simple, low cost, precise and speed spectrophotometric methods development for evaluation of sulfacetamide sodium are described. The primary approach contains conversion of sulfacetamide sodium to diazonium salt followed by a reaction with p-cresol as a reagent in the alkaline media. The colored product has an orange colour with absorbance at λmax 450 nm. At the concentration range of (5.0-100 µg.mL-1), the Beer̆ s Low is obeyed with correlation coefficient (R2= 0.9996), limit of detection as 0.2142 µg.mL-1, limit of quantification as 0.707 µg.mL-1 and molar absorptivity as 1488.249 L.mol-1.cm-1. The other approach, cloud point extraction w
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