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.
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
... 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 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 MoreThe determination hardness in water raised to rivers caused several problem in the validity of the water used depends on where determination ions concentration calcium and magnesium in salts carbonate and sulfate , this possibility of separation between of these ions and the resulting impact on concentration and determination the degree of hardness water and appreciation between the insolvent water quality . It study the effect of the impact of concentration magnesium ion in determination the quality of the water has turned out to be Mg concentration more than 60% of the total content of hardness is borderline in hardness effect the determination. Adopted in this research determination the ions in two method titration by EDTA solution and
... 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
... Show MoreMefenamic acid belongs to non-steroidal anti-inflammatory drugs that are used widely for the treatment of analgesia. Our aim from this study is to establish a new assay for the quantitative determination of mefenamic acid (MFA) in the pharmaceutical sample by two sensitive and rapid flow injection-fluorometric methods. A homemade fluorometer was used in fluorescence measurements, which using solid-state laser diode 405 and 532 nm as a source, combined with a continuous flow injection technique. The first method depends on the effect of MFA on calcein blue (CLB) fluorescence at 405 nm. Another method is a study of rhodamine-6G (Rh-6G) fluorescence after adding MFA, and recording at 532 nm. Optimum parameters as fluorescent dye concen
... Show MoreA simple, fast, inexpensive and sensitive method has been proposed to screen and optimize experimental factors that effecting the determination of phenylephrine hydrochloride (PHE.HCl) in pure and pharmaceutical formulations. The method is based on the development of brown-colored charge transfer (CT) complex with p-Bromanil (p-Br) in an alkaline medium (pH=9) with 1.07 min after heating at 80 °C. ‘Design of Experiments’ (DOE) employing ‘Central Composite Face Centered Design’ (CCF) and ‘Response Surface Methodology’ (RSM) were applied as an improvement to traditional ‘One Variable at Time’ (OVAT) approach to evaluate the effects of variations in selected factors (volume of 5×10-3 M p-Br, heating time, and temperature) on
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