A modern, rapid RP-HPLC-UV method was developed and validated in compliance with FDA and EMA guidelines for simultaneous quantification of 15 βlactam antibiotics) Ampicillin, Amoxicillin, cephalexin, cefotaxime, cefoxitin, cefamandole, cephalothin, piperacillin, penicillin, oxacillin, cloxacillin, nafcillin Carbenicillin, Mezlocillin and Dicloxacillin) in pharmaceutical formulations and pure forms. The method employs Column NEUCLEODUR C-18 (4.0 mm x 100 mm, 5µm particle size), at a temperature of thirty degrees Celsius, and the mobile phase was acetonitrile and KH2PO4 using gradient elution with a total separation time of 13 minutes, a flow rate of 1.3 ml/min, at = pH 4.5 for the buffer solution and the λ max was 220 nm. The method demonstrated a linear calibration range of 0.2- 20 µg/mL with coefficients of estimation of 0.9994 Recoveries were 100.4 - 90.86%. The chromatography approach in this study was applied to simultaneously determination of pharmaceutical compounds in commercial products
The 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 MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected opti
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions,
... Show MoreQuick and accurate quaternary mixture resolution of furosemide (FURO), carbamazepine (CARB), diazepam (DIAZ) and carvedilol (CARV) by using derivative spectrophotometric method was performed. FURO and CARV were determined by means of first (D1), second (D2), third (D3) and fourth (D4) derivative spectrophotometric methods, CARB was determined by using D1, D2, D3 derivatives, while D1 and D2 were used for the determination of DIAZ. The recommended methods were verified using laboratory prepared mixtures and then successfully applied for the pharmaceutical formulations analysis of the cited drugs. The results obtained revealed the efficiency of the proposed methods as quantitative tool of analysis of the quaternary mixture with no requirement
... 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
... Show MoreA simple analytical method was used in the present work for the simultaneous quantification of Ciprofloxacin and Isoniazid in pharmaceutical preparations. UV-Visible spectrophotometry has been applied to quantify these compounds in pure and mixture solutions using the first-order derivative method. The method depends on the first derivative spectrophotometry using zero-cross, peak to baseline, peak to peak and peak area measurements. Good linearity was shown in the concentration range of 2 to 24 µg∙mL-1 for Ciprofloxacin and 2 to 22 µg∙mL-1 for Isoniazid in the mixture, and the correlation coefficients were 0.9990 and 0.9989 respectively using peak area mode. The limits of detection (LOD) and limits of quantification (LOQ) were
... Show MoreThe present study describes employing zero-, 1st - and 2nd -order derivative spectrophotometric methods have been developed for determination of lorazepam (LORA) and clonazepam (CLON) in commercially available tablets. LORA was determined by means of 1st (D1), 2nd (D2) derivative spectrophotometric techniques using zero cross, peak height, and Peak area. D1 used for the determination of CLON by using zero cross and peak height while D2 (zero cross) was used for the determination of CLON. The method was established to be linear in concentration containing different ratios of LORA and CLON range of (20-200 mg/L) and (5-35 mg/L) at wavelength range (250 -370 nm), (210-370nm) respectively. The proposed techniques are highly sensitive, precise a
... Show MoreThe H-Point Standard Addition Method (H-PSAM) has been applied for spectrophotometric simultaneous determination of Cimetidine and Erythromycin ethylsuccinate using Bromothymol Blue (BTB) as a chromogenic complexing agent in a buffer solution at pH 5.5.
A new, Simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sulfamethoxazole (SMZ) drug in pure and dosage forms. This method based on the reaction of sulfamethoxazole (SMZ) with 1,2-napthoquinone-4-sulphonic acid (NQS) to form Nalkylamono naphthoquinone by replacement of the sulphonate group of the naphthoquinone sulphonic acid by an amino group. The colored chromogen shows absorption maximum at 460 nm. The optimum conditions of condensation reaction forms were investigated by (1) univariable method, by optimizing the effect of experimental variables (different bases, reagent concentration, borax concentration and reaction time), (2) central composite design (CCD) including the effect of
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