In-vitro drug–drug interaction studies of diltiazem with floroquinolones

Diltiazem is an established cardiovascular drug mainly used for the management of hypertension specifically for the angina pectoris. Fluoroquinolones are widely prescribed against the treatment of severe infections. In vitro relations of diltiazem with fluoroquinolones (ciprofloxacin, levofloxacin, norfloxacin, and ofloxacin) were examined using spectrophotometric and separation techniques, i.e., RP-HPLC. Diltiazem’s availabilities were observed to be predisposed highly in the presence of fluoroquinolones. To investigate the mechanism of interaction in a variety of dissolution environments, i.e., simulating body environments with regard to pH on these interactions has been studied. Moreover, complex of diltiazem–fluoroquinolones were prepared and elucidated through IR spectroscopy and confirmed by computational molecular modeling.     

Simultaneous determination of gliquidone, pioglitazone hydrochloride, and verapamil in formulation and human serum by RP-HPLC

In the present study, a reverse-phase high performance liquid chromatography method was developed, validated and applied for the simultaneous determination of gliquidone, pioglitazone hydrochloride and verapamil in tablets and human serum. Chromatographic separation was achieved on a C18 column (5 μm, 25 × 0.46 cm) with a mobile phase consisting of methanol-water-acetonitrile (80:10:10 v/v/v) with a flow rate of 0.7 mL/min and pH adjusted to 3.50 with phosphoric acid at 230 nm. Glibenclamide was used as internal standard. The experimentally derived limit of detection and limit of quantitation were determined to be 0.24, 0.93, 0.40, and 0.80, 3.11, 1.36 μg/mL for gliquidone, pioglitazone, and verapamil, respectively. There were no interfering peaks due to the excipients present in the pharmaceutical tablets. Thus, the proposed method is simple and suitable for the simultaneous analysis of active ingredients in dosage forms and human serum.     

Development and validation of stability-indicating HPLC method for the simultaneous determination of paracetamol, tizanidine, and diclofenac in pharmaceuticals and human serum

A method is described for the simultaneous determination of paracetamol, tizanidine, and diclofenac in mixtures. The method was based on HPLC separation of the three drugs followed by UV detection at 254 nm. The separation was carried out on a Hypersil ODS, C18 (250 x 4.6 mm id, 10 microm particle size) column using the mobile phase aqueous 0.2% ammonium carbonate-methanol (60 + 40, v/v) at a flow rate of 1 mL/min. The linear regression analysis data were used for the regression curve in the range of 170-10 000 ng/mL for paracetamol, 120-10 000 ng/mL for tizanidine, and 20-10 000 ng/mL for diclofenac. No chromatographic interference from tablet excipients was found. In order to check the selectivity of the proposed method, degradation studies were carried out using hydrolysis (acid, basic, and neutral), thermolysis, and oxidation. The developed method, after being validated in terms of precision, robustness, recovery, LOD, and LOQ, was successively applied to the analysis of pharmaceutical formulations and human serum.     

Stellatic acid: a new class of sesterterpenoid; X-ray crystal structure

The complete structure of a unique tricyclic sesterterpene, stellatic acid, was established by X-ray diffraction of its p-bromophenacyl ester.     

Facile LC‐UV methods for simultaneous monitoring of ciprofloxacin and rosuvastatin in API,formulations and human serum

An efficient, selective and cost‐effective liquid chromatographic assay was developed and validated for the simultaneous quantification of ciprofloxacin and rosuvastatin in Active Pharmaceutical Ingredients (API), pharmaceutical formulations and in human serum. The chromatographic system consisted of mobile phase methanol–water, 90:10 v/v at pH 3.0 adjusted with o‐phosphoric acid, pumped at 1.0 mL/min through a prepacked Purospher Star C18 (5 µm, 25 × 0.46 cm) column and effluent was monitored at the isosbestic point (255 nm) as well as at the λ_max of individual drugs (243 and 271 nm). The method was validated over a linear concentration range of 0.25–15 µg/mL for ciprofloxacin and 0.33–20 µg/mL for rosuvastatin (r² ≥ 0.999). The ranges of reliable response (limits of detection and quantitation) for ciprofloxacin were 3–15 and 9–45 ng/mL and 17–29 and 52–88 ng/mL, respectively, for rosuvastatin in all API, pharmaceutical formulations and human serum. Analytical recovery from human serum was >98% and relative standard deviation (RSD) was <2. The accuracies were 97.13–102.55 and 97.41–101.31% and precisions in RSD were 0.04–1.90 and 0.02–1.23% for ciprofloxacin and rosuvastatin, respectively. No matrix interferences, ion suppression/enhancement and carry‐over were detected. The total assay run time was less than 5 min. In another study, for optimum performance the detector was programmed for multiwavelength scanning at the absorption maxima of each component. Consequently, the linearity range was improved and limit of detection and quantitation values were down to 1–4 and 4–12 ng/mL for ciprofloxacin and 3–5 and 9–15 ng/mL for rosuvastatin, respectively. The validation parameters fitted ICH guidelines through the isosbestic and individual λ_max approach. The small sample volume and simplicity of preparation make this method suitable for use in human serum samples, pharmaceutical formulations, quality control, drug–drug interaction studies, clinical laboratories, drug research centers and forensic medical centers. Copyright © 2014 John Wiley & Sons, Ltd.     

An efficient p-tetranitrocalix[4]arene based adsorbent for the removal of carbofuran from aqueous media

Present study describes the adsorption of carbofuran (CF) from aqueous solutions using p-tetranitrocalix[4]arene based modified silica through batch and column methods. Various parameters were optimized including initial pesticide concentrations (5 mg L^?1), pH (2–10), contact time (60 min) and adsorbent dosage (30 mg). Modified silica was characterized by FT-IR and scanning electron microscope. The adsorption was further explained by Langmuir, Freundlich and Dubinin–Radushkevich (D–R) models. Moreover, adsorption kinetics and adsorption thermodynamics were also investigated. Adsorption in dynamic mode was evaluated by breakthrough volumes and the Thomas model, applying batch conditions using 30 mg of modified silica at pH 5. It has been noticed that CF removal efficiency of modified silica was 98 % as compared to bare silica (48 %). Adsorption of CF on modified silica was found to be multilayer and physical in nature. Consequently, adsorption obeys pseudo-second-order kinetic equation following external mass transfer diffusion process as the rate-limiting step. Thermodynamic parameter (ΔG, ΔS, ΔH) values suggest that the adsorption of CF is spontaneous and exothermic in nature. Thomas model rate constant k _TH (cm³ mg^?1 min^?1) and maximum solid phase concentration (q _o mg g^?1) was found to be 0.52 and 12.3, respectively, in dynamic mode.     

Mixed convection flow in vertical channel with boundary conditions of third kind in presence of heat source/sink

The effects of viscous dissipation and heat source/sink on fully developed mixed convection for the laminar flow in a parallel-plate vertical channel are investigated.The plate exchanges heat with an external fluid.Both conditions of equal and different reference temperatures of the external fluid are considered.First,the simple cases of the negligible Brinkman number or the negligible Grashof number are solved analytically.Then,the combined effects of buoyancy forces and viscous dissipation in the presence of heat source/sink are analyzed by a perturbation series method valid for small values of the perturbation parameter.To relax the conditions on the perturbation parameter,the velocity and temperature fields are solved by using the Runge-Kutta fourth-order method with the shooting technique.The velocity,temperature,skin friction,and Nusselt numbers at the plates are discussed numerically and presented through graphs.     

Determination of tryptophan in raw materials, rat brain and human plasma by RP-HPLC technique

This paper describes tryptophan (TRP) estimation in raw human plasma and rat brain by reversed-phase high-performance liquid chromatography (RP-HPLC). Estimation was carried out on a Purospher STAR C18 column using water-acetonitrile (90:10 v/v, at pH 2.7) mixture at a rate of 1.5 mL/min as mobile phase. Eluents were monitored at 273 nm by an ultraviolet detector. The method was linear (R(2) > 0.999), precise (intra-day and inter-day precision <2%) in the range of 0.25-20 μg/mL. The detection and quantification limits were 0.0144 μg/mL and 0.0437 μg/mL, respectively. In human plasma, Day 1 and Day 2 precision were 0.054-2.29% and 1.66-3.7%; whereas precisions in rat brain were 1.23-2.3% and 0.677-4.2%, respectively. The method was applied to study TRP level in human smokers and in arthritic rat brain. An efficient RP-HPLC method was developed for TRP determination that worked for clinical and research purposes.     

Preparation,characterization, and binding profile of imprinted semi-IPN cryogel composite for aluminum

Human body is greatly exposed to aluminum due to its high abundance in the environment. This nonessential metal is a threat to the patients of chronic renal disorders, as it is easily retained in their plasma and quickly accumulates in different tissues. Thus, there is great need to remove it from the aqueous environment. In this study, Al³⁺ imprinted semiinterpenetrating polymer network (semi-IPN)-based cryogel composite was prepared and applied for the purification of environmental and drinking water samples from aluminum. Poly (2-hydroxyethyl methacrylate) (pHEMA) discs were produced via cryogenic treatment and imprinted semi-IPN was introduced to the 3-(trimethoxysilyl) propyl acrylatemodified macroporous cryogel discs. The adsorption properties and selectivity of the aluminum (III) imprinted semi-IPN cryogel composite were studied in detail. The imprinted semi-IPN cryogel composite showed good selectivity towards aluminum (III) ions with the imprinting factor (IF) of 76.4 in the presence of competing copper (II), nickle (II), and iron (III) ions. The maximum adsorption capacity of 271 μmol g^-1 was obtained for aluminum (III) at pH 7.0 within 10 min using imprinted semi-IPN cryogel composite. The good selectivity and reusability of aluminum (III)-imprinted semi-IPN cryogel composite makes this material an eligible candidate for the purification of drinking water from aluminum (III) leaving important minerals remained in the water.     

Validated Method for the Simultaneous Determination of Gemifloxacin and H2‐receptor Antagonists in Bulk,Pharmaceutical Formulations and Human Serum by RP‐HPLC; In‐vitro Applications

Simple, isocratic and rapid RP‐HPLC method has been developed for the simultaneous analysis of gemifloxacin and H₂‐receptor antagonists i.e. Cimetidine, Famotidine and Ranitidine, in bulk, pharmaceutical formulation and human serum. Separation was achieved on the RP‐Mediterranea column [C18 (250 × 4.6 mm, 5 μ)] at ambient temperature using mobile phase consisting of acetonitrile: methanol: water (20:28:52 v/v/v pH 2.8 adjusted by phosphoric acid). Flow rate was 1.0 mL/min with an average operating pressure of 180 kg/cm². Gatifloxacin (GATI) was used as an internal standard (IS). Quantitation was achieved with UV detection at 221, 256 and 267 nm, respectively. Linear calibration curves, at concentration ranges of 0.05‐37.5 μgmL^‐L with a correlation coefficient of ±0.9994. The detection and quantification limits were in the ranges of 0.023‐0.250 μgmL^‐L and 0.071‐0.756 μgmL^‐L, respectively. Friedman's and Student's t‐test were applied to correlate these results. Method was validated in terms of selectivity, linearity, precision, robustness, recovery, limits of detection and quantitation and is applicable to the routine analysis of GFX and H₂‐receptor antagonists, alone or in combination.