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 simple, low cost and rapid flow injection turbidimetric method was developed and validated for mebeverine hydrochloride (MBH) determination in pharmaceutical preparations. The developed method is based on forming of a white, turbid ion-pair product as a result of a reaction between the MBH and sodium persulfate in a closed flow injection system where the sodium persulfate is used as precipitation reagent. The turbidity of the formed complex was measured at the detection angle of 180° (attenuated detection) using NAG dual&Solo (0-180°) detector which contained dual detections zones (i.e., measuring cells 1 & 2). The increase in the turbidity of the complex was directly proportional to the increase of the MBH concentration
... Show MoreA chemometric method, partial least squares regression (PLS) was applied for the simultaneous determination of piroxicam (PIR), naproxen (NAP), diclofenac sodium (DIC), and mefenamic acid (MEF) in synthetic mixtures and commercial formulations. The proposed method is based on the use of spectrophotometric data coupled with PLS multivariate calibration. The Spectra of drugs were recorded at concentrations in the linear range of 1.0 - 10 μg mL-1 for NAP and from 1.0 - 20 μg mL-1 for PIR, DIC, and MEF. 34 sets of mixtures were used for calibration and 10 sets of mixtures were used for validation in the wavelength range of 200 to 400 nm with the wavelength interval λ = 1 nm in methanol. This method has been used successfully to quant
... Show MoreA 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 MoreAn investigation was conducted for the study of extraction of metal ions using aqueous biphasic systems. The extraction of iron, zinc and copper from aqueous sulphate media at different kinds of extractants SCN− , Cl- and I- , different values of pH of the feed solution, phase ratio, concentration of metals, concentration of extractant, concentration of polymer, and concentration of salt was investigated. Atomic absorption spectrophotometer was used to measure the concentration of iron, zinc and copper in the aqueous phase throughout the experiments. The results of the extraction experiments showed the use of SCN− as extractant, pH=2.5, phase ratio=1.5, concentration of metals 1g/l, concentration of extractant 0.06 %, concentration o
... Show MoreA simple reverse-phase high performance liquid chromatographic method for the simultaneous analysis (separation and quantification) of furosemide (FURO), carbamazepine (CARB), diazepam (DIAZ) and carvedilol (CARV) has been developed and validated. The method was carried out on a NUCLEODUR® 100-5 C18ec column (250 x 4.6 mm, i. d.5μm), with a mobile phase comprising of acetonitrile: deionized water (50: 50 v/v, pH adjusted to 3.6 ±0.05 with acetic acid) at a flow rate 1.5 mL.min-1 and the quantification was achieved at 226 nm. The retention times of FURO, CARB, DIAZ and CARV were found to be 1.90 min, 2.79 min, 5.39 min and 9.56 min respectively. The method was validated in terms of linearity, accuracy, precision, limit of detection and li
... Show MoreA simple and rapid high performance liquid chromatographic with fluorescence detection method for the determination of the aflatoxin B1, B2, G1 and G2 in peanuts, rice and chilli was developed. The sample was extracted using acetonitrile:water (90:10, v/v%) and then purified by using ISOLUTE multimode solid phase extraction. After the pre-column derivatisation, the analytes were separated within 3.7 min using Chromolith performance RP-18e (100–4.6 mm) monolithic column. To assess the possible effects of endogenous components in the food items, matrix-matched calibration was used for the quantification and validation. The recoveries of aflatoxins that were spiked into food samples were 86.38–104.5% and RSDs were <4.4%. The method was
... Show MoreAn accurate and sensitive spectrophotometric method has been developed for the determination of carbamazepine (CRN.) in pure and dosage forms. The method is based on the oxidation of 2,4-dinitrophenylhydrazine (2,4-DNPHz) by potassium periodate than coupling with carbamazepine (CRN.) in alkaline medium to form a stable yellowish brown colored water-soluble dye with a maximum absorption at 485 nm. The variables that affect the completion of reaction have been carefully optimized. Beer’s law is obeyed over the concentration range of (4-50 μg.mL-1) with molar absorptivity of (6.7335×103 L.mol-1.cm1). The limit of detection was (0.1052 μg.mL-1) and Sandell’s sensitivity value was 0.0350 μg.cm-2.
... Show More