ABSTRACT
Two simple validated and highly selective methods for analysis of paracetamol, codeine, guaifenesin and pseudoephedrine or phenylephrine quaternary mixtures were developed. The first method is a high performance liquid chromatography with diode array detection method where separation was successful using Agilent C18 (150 × 4.6 mm) column, gradient elution of phosphate buffer pH 3, methanol and acetonitrile and diode-array detection at 210 nm. The second method is a HPTLC method followed by densitometric measurement of the spots at 257 nm. Separation was carried out on Merck HPTLC aluminum sheets of silica gel using methylene chloride: methanol: glacial acetic acid: ammonia (17.8: 1.68: 0.4: 0.12, v/v) mobile phase. The methods were applied successfully for analysis of both quaternary mixtures in laboratory-prepared tablets and also validated in regards to linearity, precision, accuracy, sensitivity and stability.
Subject(s)
Acetaminophen/analysis , Chromatography, High Pressure Liquid/methods , Codeine/analysis , Guaifenesin/analysis , Phenylephrine/analysis , Pseudoephedrine/analysis , Chromatography, Thin Layer/methods , Limit of Detection , Linear Models , Multi-Ingredient Cold, Flu, and Allergy Medications/analysis , Multi-Ingredient Cold, Flu, and Allergy Medications/chemistry , Reproducibility of Results , TabletsABSTRACT
This study represents simple inexpensive chromatographic determination of ciprofloxacin (CIP) and tinidazole (TIN) simultaneously in human plasma using HPLC-DAD followed by a pharmacokinetic application. C18 column was used as stationary phase with isocratic elution of a mobile phase composed of acetic acid solution (2%) and acetonitrile (85: 15, v/v) and ornidazole as internal standard (IS) with UV detection at 318â¯nm. The two drugs and the IS were separated at 6.55, 7.91 and 11.07â¯min for CIP, TIN and IS, respectively, with good selectivity and sensitivity for their analysis in presence of plasma matrix components and the drugs' metabolites. Sample preparation involved only protein precipitation without any complicated extraction procedures decreasing analysis time. For method validation, FDA regulations for analysis in biological fluids were followed. Pharmacokinetic (PK) study on six healthy volunteers was conducted after single oral dose administration of 500 and 600â¯mg of CIP and TIN, respectively. Dugs' plasma levels were followed for 12 or 72â¯h post dosing for CIP and TIN, respectively, and different PK data for the two drugs were calculated and they were comparable to the reported values demonstrating successful future application of the presented method in PK, bioequivalence and bioavailability studies.
Subject(s)
Anti-Infective Agents/blood , Ciprofloxacin/blood , Tinidazole/blood , Adult , Anti-Infective Agents/chemistry , Anti-Infective Agents/pharmacokinetics , Chromatography, High Pressure Liquid/economics , Chromatography, High Pressure Liquid/methods , Ciprofloxacin/chemistry , Ciprofloxacin/pharmacokinetics , Drug Combinations , Drug Stability , Humans , Limit of Detection , Linear Models , Male , Reproducibility of Results , Tinidazole/chemistry , Tinidazole/pharmacokineticsABSTRACT
Two novel combination therapies for the treatment of benign prostatic hyperplasia were analyzed using simple and enhanced spectrofluorimetric methods based on derivative and derivative ratio techniques. The two combinations contained tamsulosin hydrochloride (TAM) as a minor component with tolterodine tartrate (TOL) or solifenacin succinate (SOL). The fluorescence of the three drugs under study was measured in methanolic water solution. For the TAM and SOL mixture, successful resolution between both drugs was achieved by derivative manipulation of both ratio and zero-order emission spectra with good linearity in the ranges of 0.75-3.50 and 2.5-15.0 µg ml-1 for TAM and SOL, respectively. Extensive emission spectral overlap was observed for the TAM and TOL mixture. Therefore, only derivative application of the ratio emission spectra resolved such overlap and quantitated TAM and TOL simultaneously in the ranges 0.75-3.50 and 2.5-20.0 µg ml-1 for TAM and TOL, respectively. Optimization of various experimental parameters that affected the fluorescence intensity of the three drugs was performed. Successful application of all proposed methods was achieved for analysis of the two drugs in each combination therapy in their laboratory-prepared mixtures and dosage forms with good accuracy and precision.
Subject(s)
Prostatic Hyperplasia/drug therapy , Solifenacin Succinate/therapeutic use , Sulfonamides/therapeutic use , Tolterodine Tartrate/therapeutic use , Dose-Response Relationship, Drug , Drug Therapy, Combination , Humans , Male , Molecular Structure , Solifenacin Succinate/chemistry , Spectrometry, Fluorescence , Sulfonamides/chemistry , Tamsulosin , Tolterodine Tartrate/chemistryABSTRACT
A validated and selective high-performance thin-layer chromatography (HPTLC) method was developed for the analysis of mixures of tamsulosin hydrochloride (TAM) with either tolterodine tartrate (TOL) or solifenacin succinate (SOL) in bulk drug and in combined dosage forms. The proposed method is based on HPTLC separation of the three drugs followed by densitometric measurements of their spots at 224 nm. Separation was carried out on Merck HPTLC aluminum sheets of silica gel 60 F254 using ethyl acetate-methanol-ammonia (6:4:0.05, v/v) as mobile phase. The linear regression analysis data were used for the regression line in the range of 0.1-0.7, 0.4-4 and 1-6 µg band-1 for TAM, TOL and SOL, respectively. The proposed method was validated and successfully applied for the analysis of their pharmaceutical formulations and laboratory-prepared mixtures containing the two bicomponent combinations. The method was validated and showed good performances in terms of linearity, sensitivity, precision, accuracy and stability.
