Classical versus chemometrics tools for spectrophotometric determination of fluocinolone acetonide, ciprofloxacin HCl and ciprofloxacin impurity-A in their ternary mixture.

Green, simple, accurate and robust univariate and chemometrics assisted UV spectrophotometric approaches have been adopted and validated for concurrent quantification of fluocinolone acetonide (FLU), ciprofloxacin HCl (CIP) together with ciprofloxacin impurity-A (CIP imp-A) in their ternary mixture. Double-divisor ratio spectra derivative (DDRD) method has been used for determination of FLU. On the other hand, the first (D1) and second (D2) derivative approaches have been applied for the quantification of CIP and CIP imp-A, respectively. For the ratio difference (RD), derivative ratio (DR), and mean centering of ratio spectra (MC) methods, CIP and its impurity A have been simultaneously determined. The acquired calibration plots were linear over the concentration range of 0.6-20.0 µg/mL, 1.0-40.0 µg/mL and 1.0-40.0 µg/mL for fluocinolone acetonide, ciprofloxacin HCl, and ciprofloxacin impurity-A, respectively. The chemometrics methods namely; partial least squares (PLS) and artificial neural networks (ANN) were used for the concurrent determination of the three adopted components via using twenty-five mixtures as calibration set and fifteen mixtures as validation one. The investigated approaches were validated in accordance with International Council for Harmonisation (ICH) guidelines, and statistically compared with the official ones. The proposed methods were acceptably applied to the examination of FLU and CIP in their pure powders and pharmaceutical ear drops.

Two fabricated carbon paste electrodes for novel potentiometric determination of probenecid in dosage form and human plasma.

Solid contact ion selective electrodes are extensively utilized owing to their marvelous performance over traditional liquid contact ones. The main drawback of those solid contact electrodes is aqueous layer formation which affects their constancy. Herein and to overcome this common drawback, a carbon paste electrode containing poly(3,4-ethylenedioxythiophene) was constructed and used for determination of probenecid at variant pH values. This modification decreased the potential drift down to 0.8 mV/h and improved its stability over 30 days. A Nernstian slope of - 57.8 mV/decade associated with a linear range of 1.0 × 10-6-1.0 × 10-2 mol/L was obtained. The modified carbon paste electrode successfully detected up to 8.0 × 10-7 mol/L probenecid. Results of this modified carbon paste electrode were also compared to unmodified one.

Smart spectrophotometric methods for stability assessment of two co-formulated antigout drugs.

Simple, sensitive and accurate stability indicating spectrophotometric methods have been developed for the simultaneous determination of probenecid, colchicine as well as colchicine degradation product in their ternary mixture. Probenecid was firstly assayed using the double divisor ratio spectra derivative method. On the other hand, three spectrophotometric methods, namely: ratio difference, derivative ratio and mean centering of ratio spectra, have been suggested for the simultaneous quantification of colchicine and its degradation product. The obtained calibration curves were linear at 2.5-30.0 µg/mL, 0.5-25.0 µg/mL and 1.0-13.0 µg/mL for probenecid, colchicine and colchicine degradation product, respectively. The investigated methods were validated in accordance with the International Council for Harmonisation guidelines and were effectively used for quantification of probenecid and colchicine in their bulk powders and combined pharmaceutical dosage form.

Two Validated Chromatographic Methods for Determination of Ciprofloxacin HCl, One of its Specified Impurities and Fluocinolone Acetonide in Newly Approved Otic Solution.

Two sensitive, selective and precise chromatographic methods have been established for concomitant quantification of ciprofloxacin HCl (CIP), fluocinolone acetonide (FLU) along with ciprofloxacin impurity A (CIP-imp A). The first method was thin-layer chromatography (TLC-densitometry) where separation was accomplished using TLC silica plates 60 G.F254 as a stationary phase and chloroform-methanol-33%ammonia (4.6:4.4:1, by volume) as a developing system. The obtained plates were scanned at 260 nm over concentration ranges of 1.0-40.0, 0.6-20.0 and 1.0-40.0 µg band-1 for CIP, FLU and CIP-imp A, respectively. The second method was based on high-performance liquid chromatography using a Zorbax ODS column (5 µm, 150 × 4.6 mm i.d.) where adequate separation was achieved through a mobile phase composed of phosphate buffer pH 3.6-acetonitrile (45:55, v/v) at flow rate 1.0 mL min-1 with ultraviolet detection at 254 nm. Linear regressions were obtained in the range of 1.0-40.0 µg mL-1 for CIP, 0.6-20.0 µg mL-1 for FLU and 1.0-40.0 µg mL-1 for CIP-imp A. The suggested methods were validated in compliance with the International Conference on Harmonization guidelines and were successfully applied for determination of CIP and FLU in bulk powder and newly marketed otic solution.

Stability-Indicating Chromatographic Methods for the Simultaneous Determination of Probenecid and Colchicine in Their Combined Tablet.

Two stability-indicating chromatographic methods have been established and validated for concurrent determination of probenecid (PRO), colchicine (COL) along with the degradation product of colchicine (COL deg). PRO and COL were exposed to a stress stability study, which includes acidic, alkaline, oxidative, photolytic and thermal degradations. Chromatographic methods included the use of thin layer chromatography (TLC-densitometry) and high performance liquid chromatography (HPLC). In the first method, separation was achieved by using aluminum TLC plates that were precoated with silica gel G.F254 as the stationary phase and ethyl acetate-methanol-33%ammonia (8:1:1, by volume) as a mobile phase. The obtained chromatograms were scanned at 254 nm. The second method was based on HPLC using a RP- C18 column with isocratic elution. Good separation was obtained through a mobile phase comprised of phosphate buffer pH 5-acetonitrile (70:30, v/v) at a flow rate of 1.0 mL min-1 and ultraviolet detection at 254 nm. Different parameters affecting efficiency of the two methods were studied accurately for optimum separation of the three cited components. The suggested methods were validated according to the International Conference on Harmonization (ICH) guidelines and were applied for bulk powder and commercial tablets.