High‐Performance Liquid Chromatographic Determination of Parecoxib in Human Plasma and Pharmaceutical Formulations

Abstract

A simple and sensitive RP‐HPLC method for the determination of parecoxib (PXB) in human plasma and pharmaceutical formulations has been developed and validated. The separation of PXB and the internal standard, ibuprofen (IBF) was achieved on a CLC C₁₈ (5 μ, 25 cm×4.6 mm i.d.) column using UV detector at 200 nm. The mobile phase consisted of acetonitrile‐water (92:8 v/v). The linear range of detection was found to be 0.9–18.4 µg/ml (r=0.9985). Intra‐ and inter‐day assay relative standard deviations were observed to be less than 0.3%. The method has been applied successfully for the determination of PXB in spiked human plasma and pharmaceutical preparations. Analytical parameters were calculated and complete statistical evaluation is incorporated.     

High‐Performance Liquid Chromatography Determination of Latanoprost in Pharmaceutical Formulations using UV Detection

Abstract

A simple, fast, and accurate high‐performance liquid chromatography (HPLC) method was developed to determine latanoprost in pharmaceutical formulations. The drug was chromatographed on a C₁₈ column. Eluents were monitored at a wavelength of 210 nm using a mixture of acetonitrile and 0.05 M potassium phosphate buffer pH 3.0 (70:30, (v/v). A linear response (r>0.9998) was observed in the range of 10.0–90.0 µg mL^?1. The method showed good recoveries (average 100.4%) and the relative standard deviations intra‐ and inter‐day were ≤1.0%. The method can be used for quality control assay of latanoprost in raw materials as well as in pharmaceutical formulations.     

RP‐HPLC Method for the Determination of Tenofovir in Pharmaceutical Formulations and Spiked Human Plasma

Abstract

A simple reverse‐phase high‐performance liquid chromatographic method for the determination of tenofovir disoproxil fumarate (TDF) in pharmaceutical formulations and human plasma samples has been developed and validated. Piroxicam (PRX) was used as an internal standard. The assay of the drug was performed on a CLC C₁₈ (5 μ, 25 cm×4.6 mm i.d.) with UV detection at 259 nm. The mobile phase consisted of acetonitrile–water mixture in the ratio of 75∶25, and a flow rate of 1 ml/min was maintained. The standard curve was linear over the range of 0.2–10 µg/ml (r ²=0.9966). Analytic parameters have been evaluated. Within‐day and between‐day precision as expressed by relative standard deviation was found to be less than 2%. The method has been applied successfully for the determination of TDF in spiked human plasma samples and pharmaceutical formulations.     

Application of Internal Standard for Micro Extraction– Spectrophotometric Determination of Bismuth in Pharmaceutical Formulations

 A micro extraction – spectrophotometric procedure is developed for the determination of bismuth in pharmaceutical formulations. The procedure is based on the extraction of tetraiodobismuthate(III) ion paired with benzyltributylammonium cation into chloroform. The application of Nile Blue as internal standard (IS) enabled good analytical performance for micro-scale analysis. The ratio between the absorbances measured at 491 nm (bismuth complex) and at 632 nm (IS) was taken as the analytical signal. The procedure was carried out in Eppendorf tubes, lowering significantly the use of reagents and the volume of organic solvent. In the calibration range up to 60 mgċl⁻¹, the linear regression coefficient was 0.9999, the CV for 15 mgċl⁻¹ and for 50 mgċl⁻¹ Bi were 1.6% and 0.7% respectively. The results obtained in the analysis of pharmaceutical formulations were in good agreement with the results of EDTA titration method. Received November 25, 1999. Revision February 14, 2000.     

Quantitative Determination of Nadolol in Tablets by High‐Performance Liquid Chromatography and UV‐Derivative Spectrophotometry

Abstract

High‐performance liquid chromatographic (HPLC) and UV derivative spectrophotometric (UVDS) methods were developed and validated for the quantitative determination of nadolol in tablets. The HPLC method was performed on a C18 column with fluorescence detection. The excitation and emission wavelengths were 230 and 300 nm, respectively. A mobile phase composed by acetonitrile‐water containing 0.1% triethylamine (15∶85 v/v) and pH adjusted to 4.6 with formic acid was used. The UVDS method was performed taken a signal at 279.5 nm. The correlation coefficient (r) obtained for both methods was 0.9999. The proposed methods are simple, precise, accurate, and can be used in routine analysis.     

Stability-Indicating Liquid Chromatography–Spectrophotometric UV Method for the Simultaneous Determination of Marbofloxacin,Dexamethasone and Clotrimazole in a Liquid Pharmaceutical Dosage Form

A novel, simple and reliable reversed-phase liquid chromatography (LC)–spectrophotometric UV stability-indicating method was developed and validated for the simultaneous assay of marbofloxacin, clotrimazole and dexamethasone acetate in the presence of their impurities and degradation products in a pharmaceutical formulation for veterinary use. A C18 (75 × 4.6 mm, 4 µm) column was used with an acetonitrile–ammonium acetate mixture as mobile phase delivered with gradient elution. A diode-array detection was used in the 200–400 nm range and the detection wavelength was set at 260 nm. Validation carried out on the pharmaceutical dosage form, according to Veterinary International Conference on Harmonization guidelines, demonstrated excellent specificity, linearity, precision, accuracy and robustness. Excellent specificity with respect to vehicle and degradation products obtained after forced degradation (i.e., oxidation, acid, alkaline and thermal degradation) was demonstrated. As for linearity, the LC–UV assay method is applicable in the 0.180–0.420 mg mL^?1 concentration range for marbofloxacin (r ² = 0.99), 0.060–0.140 mg mL^?1 for dexamethasone acetate (r ² = 0.97) and 0.600–1.400 mg mL^?1 for clotrimazole (r ² = 0.98). Very good repeatability (RSD < 0.8 %) and inter-day precision (RSD < 2.5 %) were observed for all analytes. Accuracy was in the 93–104 %, 98–111 % and 99–108 % confidence interval (95 %) for marbofloxacin, dexamethasone acetate and clotrimazole, respectively. The variations (±20 %) of mobile phase flow rate and pH, and oven column temperature did not exhibit an impact on the analyte content accuracy, demonstrating the robustness of the method. The LC–UV method here developed and validated may be used routinely for quality control.     

Development and Validation of Spectrophotometric Methods for the Determination of Cefetamet in Pharmaceutical Dosage Forms

Two simple and sensitive spectrophotometric methods for the determination of cefetamet in either pure form or in its pharmaceutical formulations were described. The method Ⅰ is based on the interaction of 3-methylbenzo[d]- thiazolin-2-one hydrazone （MBTH） with cefetamet in the presence of freshly prepared ferric chloride in a neutral medium. The resulting blue colored product has λmax at 628 nm. The method Ⅱ describes the reduction of ferric ion by the drug to ferrous ion followed by a complex formation reaction with 1,10-phenanthroline （1,10-phen） to form an orange red colored chromogen exhibiting 2max at 510 nm. The products are stable for more than 5 and 8 h respectively. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed methods. Both methods are highly reproducible and have been applied to a wide variety of pharmaceutical preparations and the results are comparable with those of official methods.     

Development and Validation of High‐Performance Liquid Chromatographic Method for Estimation of Lercanidipine in Rabbit Serum

Abstract

A new, simple, and sensitive reverse‐phase liquid chromatographic method was developed and validated for the estimation of Lercanidipine hydrochloride in rabbit serum using UV detector under isocratic conditions. After subjecting serum to simple and efficient one‐step extraction procedure, 100 µl of sample was injected onto high‐performance liquid chromatography system. The detector response was linear in the concentration range of 25–1000 ng/ml. The developed method was validated as per standard guidelines. Validation demonstrated accuracy, precision, and selectivity of the proposed method. The drug was found to be stable under various processing and storage conditions.     

Liquid Chromatographic Method for Determination of Free and Niosome‐Entrapped Nimodipine in Mouse Plasma and Different Tissues

Abstract

A rapid HPLC method for the quantification of nimodipine in mouse plasma and tissues has been developed in this study, with simple procedure of sample preparation by one‐step protein precipitation. The results of HPLC analysis indicated that linear calibration curves were obtained over the concentration range 0.10–10.00 µg/ml for plasma, 0.10–20.00 µg/g for heart, liver, spleen, kidneys, and brain, and 1.00–200.00 µg/g for lung, respectively. The desirable precision and accuracy were achieved, both intraday and interday for plasma and tissue homogenates. Thus, this newly developed procedure was successfully applicable for determination of nimodipine in mouse plasma and tissues following intravenous administration of free and novel niosome‐entrapped nimodipine.     

Liquid Chromatographic Resolution of the Enantiomers of Metoprolol and Carvedilol in Pharmaceutical Formulations by use of Marfey’s Reagent and its Variants

JPC – Journal of Planar Chromatography – Modern TLC - A simple and rapid method has been established for indirect separation of the enantiomers of (R,S)-metoprolol and (R,S)-carvedilol...     

Isobaric Binary and Ternary Vapor–Liquid Equilibrium for the Mixture of n-Hexane,Methylcyclopentane and N-Methylpyrrolidone

Journal of Solution Chemistry - The vapor–liquid phase equilibrium (VLE) data for binary systems of: n-hexane?+?methylcyclopentane, n-hexane?+?N-methylpyrrolidone...     

Development and Validation of a Chiral Liquid Chromatographic Method for Quantitative Determination of (+)-OTX015 in (−)-OTX015

A simple, rapid and robust enantioselective method was developed and validated for the quantitation of OTX015 enantiomers [(−)-OTX015 and (+)-OTX015] with ultrahigh-performance liquid chromatography (UHPLC) as per ICH guidelines. The active [(−)-OTX015] and inactive [(+)-OTX015] enantiomers were resolved on a Chiralpak-IA column using methanol consisting of 0.1 % diethyl amine at a flow rate of 1.0 mL min⁻¹. The resolution between the enantiomers was found to be more than 3.7 in the optimized method. The developed method was extensively validated and proven to be robust. The calibration curve for (+)-OTX015 showed excellent linearity over the concentration range of 10–100 µg mL⁻¹. The limit of detection and the limit on quantitation for (+)-OTX015 were 5 and 10 µg mL⁻¹, respectively. The recovery for (+)-OTX015 ranged between 100.7 and 102.5 % in the bulk drug sample of (−)-OTX015. The proposed method was found to be suitable and accurate for quantitative determination of (+)-OTX015 in bulk drug.

     

Study on the Application of Gibberellin for the Spectrophotometric Determination of Arsenic,Phosphorus,Silicon and Germanium

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FT‐IR Spectrophotometric Analysis of Chromium (Tris) Picolinate and its Pharmaceutical Formulations

Abstract

A Fourier transform infrared (FT‐IR) spectrometric method was developed for the rapid, direct measurement of chromium (tris) picolinate [Cr(pic)₃] in different pharmaceutical products. Conventional KBr potassium bromine spectra were compared for best determination of active substance in drug preparations. Lambert‐Beer's law and two chemometric approaches, partial least squares (PLS) and principal component regression (PCR+) methods, were used in data processing.     

PLS Regression in the Spectrophotometric Data for the Simultaneous Determination of Levodopa and Carbidopa in Pharmaceutical Preparations by Using an Enzymatic Stopped‐Flow FIA Technique

Abstract

An enzymatic stopped‐flow‐injection analysis is proposed for simultaneous determination of levodopa and carbidopa in pharmaceutical preparations. The dopaquinones obtained after the oxidation catalized by the enzyme were measured by spectrophotometric method. A reduced calibration matrix based on a central composite experimental design was built and Partial Least Squares (PLS) was applied on the spectral data after reaction with the enzyme. The LOD was 0.015 and 0.0028 mg ml^?1, respectively and the sample throughput was 22.5 h^?1. The proposed method was applied to pharmaceutical preparations and the results are in close agreement with pharmacopeial method. The recovery study and results were satisfactory.     

1, 1‐Dianthrimide as a Reagent for the Spectrophotometric Determination of Boron

Abstract

The optimum conditions for the formation of the blue 1:1 complex by the reaction of 1, 1‐dianthrimide and boric acid in 95% by weight sulfuric acid have been determined. The effect of certain diverse ions are reported. The procedure is applicable to the determination of 1 to 10 μ of boron.     

High-Performance Liquid Chromatographic Determination of the Metabolites of the Potato Glycoalkaloids, α-Chaconine and α-Solanine,in Potato Tubers and Potato Products

Abstract

A high-performance liquid chromatographic method has been developed to separate and quantify the metabolites, γ-chaconine, β₁-and β₂-chaconine, γ-solanine and β₂-solanine, of the potato gly-coalkaloids α-chaconine and α-solanine in potatoes and potato products. A carbohydrate analysis column and a solvent system of tetrahydrofuran-water-acetonitrile (55:8:37) were employed for the separation. Flow rate was 1.1 ml/min and the compounds were monitored at 215 nm. β₂-chaconine (0.63 mg to 29.75 mg/100 g dried weight) was present in all samples whereas the other glycosides of α-chaconine were only detectable in the animal feed products. It appears that some of the animal feeds may contain trace amounts of γ-solanine and an unknown which maybe β₁-solanine. Limit of detection for all glycosides was 0.05 μg/μl. Elution time for all the lower glycosides of α-chaconine was 8 min versus 16 min for the α-solanine group. These metabolic compounds were confirmed using thin-layer chromatography.     

Flow‐Injection Spectrophotometric Determination of N‐acetylcysteine in Pharmaceutical Formulations with On‐Line Solid‐Phase Reactor Containing Zn(II) Phosphate Immobilized in a Polyester Resin

Abstract

A flow‐injection spectrophotometric procedure was developed for determining N‐acetylcysteine in pharmaceutical formulations. The sample was dissolved in deionized water and 400 µl of the solution was injected into a carrier stream of 1.0×10^?2 mol l^?1 sodium borate solution. The sample flowed through a column (70 mm length×2.0 mm i.d.) packed with Zn₃(PO₄)₂ immobilized in a polymeric matrix of polyester resin and Zn(II) ions were released from the solid‐phase reactor because of the formation of the Zn(II) (N‐acetylcysteine)₂ complex. The mixture merged with a stream of borate buffer solution (pH 9.0) containing 5.0×10^?4 mol l^?1 Alizarin red S and the Zn(II)Alizarin red complex formed was measured spectrophotometrically at 540 nm. The analytical curve was linear in the N‐acetylcysteine concentration range from 3.0×10^?5 to 1.5×10^?4 mol l^?1 (4.9 to 24.5 µg ml^?1) with a detections limit of 8.0×10^?6 mol l^?1 (1.3 µg ml^?1). The relative standard deviations (RSDs) were smaller than 0.5% (n=10) for solutions containing 5.0×10^?5 mol l^?1 (8.0 µg ml^?1) and 8.0×10^?5 mol l^?1 (13.0 µg ml^?1) of N‐acetylcysteine, and the analytical frequency was 60 determinations per hour. A paired t‐test showed that all results obtained for N‐acetylcysteine in commercial formulations using the proposed flow‐injection procedure and a comparative procedure agreed at the 95% confidence level.     

Prediction of the Properties of a Binary Surfactant Mixture of Arlacel‐165 and Myrj‐59 in Aqueous System

Foamability and foam stability, emulsifying power, surface tension, and interfacial tension were investigated for different ratios of binary surfactant system of Arlacel‐165 (glyceryl stearate (and) PEG‐100 stearate) and Myrj‐59 (polyoxyethylene 100 stearate). Among all the ratios tested for their foaming power and foamabilty, the ratios 8:2, 5:5, 4:6, 2:8, and 1:9 of Arlacel‐165 and Myrj‐59 showed the best results. At these ratios, the foaming power and foamability was found to be 100%. The surfactants having foam stability more than 50% can be considered as metastable and those less than 50% are considered as low‐stability foams. In case of surface tension and interfacial tension property measurements, 8:2 and 9:1 showed the best results. At 8:2 and 9:1 of Arlacel‐165 and Myrj‐59, the surface tension was found to be 37.7 dynes/cm and 1.33 dynes/cm respectively at 30°C ambient temperature. Also, 7:3 of this binary mixture was found to exhibit the best emulsifying power among all the ratios tested. At 30°C, the emulsifying property of the binary mixture was 6 hours.