Direct Enantiomeric Resolution of Betaxolol with Application to Analysis of Pharmaceutical Products

2006 ◽  
Vol 1 ◽  
pp. 117739010600100 ◽  
Author(s):  
Mohamed M. Hefnawy ◽  
Maha A. Sultan ◽  
Mona M. Al-Shehri
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Ophthalmic Solution ◽  
High Performance Liquid Chromatographic ◽  
Pharmaceutical Products ◽  
Hplc Method ◽  
Enantiomeric Resolution ◽  
Relative Standard ◽  
The Stability ◽  
Liquid Chromatographic

A high-performance liquid chromatographic (HPLC) method has been developed for the separation and determination of S- and R-enantiomers of betaxolol in tablets and ophthalmic preparations. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with fluorescence detection at excitation/emission wavelengths 275/305 nm. The polar ionic mobile phase (PIM) consists of methanol-glacial acetic acid-triethylamine, (100:0.020:0.025, v/v/v) has been used at a flow rate of 1.5 ml/min. All analytes with S-(-)-atenolol as internal standard were conducted at ambient temperature. The method is highly specific where another coformulated compounds did not interfere. The stability of betaxolol enantiomers under different degree of temperature also studied. The results showed that it is stable for at least 7 days at 70°C. The method validated for its linearity, accuracy, precision and robustness. Experimental design was used during validation to evaluate method robustness. Using the chromatographic conditions described, S- and R-betaxolol were well resolved with mean retention times of 11.3 and 12.6 min, respectively. Linear response (r > 0.997) was observed over the range of 10-500 ng/ml of betaxolol enantiomers, with detection limit of 5 ng/ml. The recoveries of S- and R-betaxolol from tablets and ophthalmic preparation ranged from 97.4 to 101.4% and 98.0 to 102.0%, respectively. The mean relative standard deviation (R.S.D.%) for both enantiomers were 1.1-1.4% and 1.3-1.7% in tablets and ophthalmic solution, respectively.

scholarly journals A Simple and Sensitive HPLC Method for Simultaneous Analysis of Nabumetone and Paracetamol in Pharmaceutical Formulations

2011 ◽  
Vol 8 (s1) ◽  
pp. S41-S46
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna ◽  
Dillipkumar Sahoo
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Aqueous Acetic Acid ◽  
Linear Calibration ◽  
Acceptance Range ◽  
Liquid Chromatographic

This paper describes a high-performance liquid chromatographic method for simultaneous estimation of nabumetone and paracetamol in binary mixture. The method was based on RP-HPLC separation and quantitation of the two drugs on hypersil C-18 column (250 mm × 4.6 mm) using a mobile phase consisting of acetonitrile and 0.05% aqueous acetic acid (70:30v/v) at flow rate of 1 mL min-1. Quantitation was achieved with PDA detector at 238 nm based on peak area with linear calibration curves at concentration ranges 5-25 µg mL-1for both the drugs. Naproxen sodium was used as internal standard. The method has been successively applied to pharmaceutical formulation. No chromatographic interference from the tablet excipients was found. The method was validated in terms of precision, robustness, recovery and limits of detection and quantitation. The intra and inter-day precision and accuracy values were in the acceptance range as per ICH guidelines.

scholarly journals Development of a New High-Performance Liquid Chromatographic Method for the Determination of Ceftazidime

2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Calibration Graph ◽  
Raw Material ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

Liquid-chromatographic measurement of nitrazepam in plasma.

1982 ◽  
Vol 28 (7) ◽  
pp. 1478-1481 ◽  
Author(s):  
H Kelly ◽  
A Huggett ◽  
S Dawling
Keyword(s):  
Complete Resolution ◽  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Small Sample ◽  
Ultraviolet Detector ◽  
Liquid Chromatographic Method ◽  
Chromatographic Measurement ◽  
The Stability ◽  
Liquid Chromatographic

Abstract In this simple and rapid "high-performance" liquid-chromatographic method for determining nitrazepam in plasma, serum, or whole blood, the sample at pH 7.4 is extracted into diethyl ether with an internal standard (prazepam), chromatographed, and detected at 280 nm with a fixed-wavelength ultraviolet detector. A specimen, together with standards and a quality control, can be analyzed in duplicate within 90 min. The limit of sensitivity is 5 micrograms/L (nitrazepam and 7-acetamidonitrazepam) and 50 micrograms/L (7-aminonitrazepam), and no interferents have been found. This method has the advantages of a small sample requirement and complete resolution of nitrazepam and the above-mentioned major metabolites. We have used this method for analysis of therapeutic and overdose concentrations of nitrazepam, and to investigate the stability of the drug in blood.

scholarly journals Gas Chromatographic Analysis of Capsaicin in Gochujang

2008 ◽  
Vol 91 (2) ◽  
pp. 387-391 ◽  
Author(s):  
Jaeho Ha ◽  
Kyu-Jai Han ◽  
Ki-Jin Kim ◽  
Seung-Weon Jeong
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Calibration Graph ◽  
Internal Diameter ◽  
Determination Limit ◽  
Flame Ionization ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A sensitive, precise, and specific gas chromatographic (GC) method was developed for the analysis of capsaicin in Gochujang and validated by comparing with a column high-performance liquid chromatographic (HPLC) method (AOAC 995.03). The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The GC separation was performed on a (5 phenyl)-methylpolysiloxane column [length 30 m, internal diameter (id) 250 μm, film thickness 0.25 μm] followed by flame ionization detection. The conditions of temperature programming were initially 220Cfor 1min, rampat5C/minto270C, and hold for 10 min. The recovery of capsaicin in Gochujang was more than 92, and the detection limit and lower determination limit of the GC analysis were 1.0 and 5.0 μg/g, respectively. The calibration graph for capsaicin was linear from 1 to 250 μg/mL for GC and 0.5 to 50 μg/mL for HPLC. The interday and intraday precisions (relative standard deviations) were <4.02.

scholarly journals Development and Validation of a Micellar High-Performance Liquid Chromatographic Method for Determination of Risedronate in Raw Material and in a Pharmaceutical Formulation: Application to Stability Studies

2010 ◽  
Vol 93 (4) ◽  
pp. 1228-1235 ◽  
Author(s):  
Mohamed Walash ◽  
Mohamed Metwally ◽  
Manal Eid ◽  
Rania El-Shaheny
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Sodium Dodecyl ◽  
Oxidative Degradation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Raw Material ◽  
Forced Degradation ◽  
The Stability ◽  
Liquid Chromatographic

Abstract A micellar HPLC method was developed for analysis of the antiosteoporosis drug risedronate. The analysis was carried out using a 250 4.6 mm id, 5 m particle size C18 Waters Symmetry column. The mobile phase consisted of 0.02 M sodium dodecyl sulfate + 0.3 triethylamine + 10 n-propanol, prepared in 0.02 M orthophosphoric acid. The pH of the mobile phase was adjusted to pH 6.0, and it was pumped at a flow rate of 0.7 mL/min with UV detection at 262 nm. The method showed good linearity in the range of 280 g/mL, with an LOD of 0.40 g/mL (1.31 106 M) and an LOQ of 1.21 g/mL. The suggested method was successfully applied for the analysis of risedronate in raw material and a tablet formulation, with average recoveries of 99.91 1.30 and 101.52 0.30, respectively. The stability-indicating capability of the proposed method was proved using forced degradation. By changing the pH of the mobile phase to 4.0, the oxidative degradation product could be separated from risedronate.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

High-Performance Liquid-Chromatographic Measurement of Plasma Creatinine in Newborns

1992 ◽  
Vol 38 (1) ◽  
pp. 101-103 ◽  
Author(s):  
Paul H Scott
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Exchange Chromatography ◽  
Plasma Creatinine ◽  
Standard Curve ◽  
Analytical Recovery ◽  
Liquid Chromatographic

Abstract This HPLC method for measuring plasma creatinine is based on cation-exchange chromatography and is particularly suitable for use with specimens from babies. A short chromatographic run is performed after simple protein precipitation with zinc sulfate and addition of an internal standard, N-methylnicotinamide. The standard curve for the method is linear up to 200 mumol/L, and analytical recovery of added creatinine is between 101% and 103%. Between-batch precision (CV) is less than 3% for mean creatinine values of 103 and 164 mumol/L. The method is free of interference from other metabolic components and drugs commonly used in neonates in routine clinical practice. Using specimens from neonates, I compared this method with a routinely used automated alkaline picrate method (from Randox Labs., performed on a Cobas MIRA analyzer). Linear-regression analysis yielded a correlation coefficient of 0.90, a slope of 1.00, and an intercept of +0.8 mumol/L. This HPLC method for creatinine should be of use in those circumstances where the alkaline picrate method is known to produce dubious results; however, the latter method is probably more suitable for routine use.

Analysis of spectinomycin in fermentation broth by reversed-phase chromatography

2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Hong Yan ◽  
Pei Xu ◽  
Hai Huang ◽  
Juan Qiu
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Fermentation Broth ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Standard Curve ◽  
Relative Standard ◽  
Liquid Chromatographic

AbstractA pre-column derivatized high-performance liquid chromatographic (HPLC) method with ultraviolet-visible detection was developed to measure the concentrations of spectinomycin in fermentation broth. Derivatization reagents, 2,4-dinitrophenylhydrazine in acetonitrile (5 mg mL−1) and trifluoroacetic acid in acetonitrile (0.8 mol L−1), were added to an aliquot of the fermentation broth, and the mixture was incubated for 60 min at 70°C. The resulting derivative was separated from other compounds by isocratic elution in a reversed-phase column Zorbax SB-C18 (250 mm × 4.6 mm, 5 µm). Mobile phase consisted of acetonitrile, tetrahydrofuran, and water (φ r = 40: 35: 25) and the flow rate was 1.0 mL min−1. The detection wavelength was 415 nm. The standard curve for spectinomycin sulfate was linear with correlation coefficients of 0.9997 in the range of 25 µg mL−1 to 600 µg mL−1. The relative standard deviation values ranged from 0.43 % to 2.18 % depending on the concentration of samples. The average recovery was 101.5 %. The limit of detection was 50 ng mL−1.

scholarly journals Determination of Ketoconazole in tablets by using three different methods

2012 ◽  
Vol 4 ◽  
Author(s):  
Biljana Gjorgjeska
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Analytical Work ◽  
Liquid Chromatographic ◽  
Hplc Analyses

Ketoconazole has been widely used as an antifungal drug  that is formulated as tablets, cream and over­the­counter ketoconazole shampoo. The aim of this research was to study and to standardize an ultraviolet spectrophotometric (UVS) method, potentiometric  and a high  performance  liquid  chromatographic  (HPLC) method  for  the determination  of ketoconazole in commercially available Oromycosal® tablets. These three methods were compared and discussed with respect to  their  sensitivity,  selectivity  and ready­applicability  in  routine  analytical  work.   Absorption  spectra and spectrophotometric determinations were carried out on the UVS spectrophotometer. Investigated concentrations were in range from  0.003 to  0.02mg?dm­3. The absorbance was measured at 224  nm.  In potentiometric  titrations  glass  and saturated (KCl) calomel electrode were used. HPLC analyses of ketoconazole were carried in the presence of econazole as internal standard. It can be concluded that the described methods are simple, fast and reliable for determination of ketoconazole in pharmaceutical preparations. The preparation of the samples is easy, the excipients do not  interfere in the methods, so they can be used in routine quality control analysis.

Paired-Ion Chromatography and High Performance Liquid Chromatography of Labetalol in Feeds

1980 ◽  
Vol 63 (6) ◽  
pp. 1262-1265
Author(s):  
Edward R Townley ◽  
Bruce Ross
Keyword(s):  
Acetic Acid ◽  
Ion Chromatography ◽  
High Performance ◽  
Blocking Agent ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Beta Adrenoceptor ◽  
Insoluble Material ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method using reverse phase paired-ion chromatography and ultraviolet detection at 280 nm has been developed to determine labetalol, an alpha and beta adrenoceptor blocking agent, in Purina No. 5001 rodent chow. The method is simple and rapid, and demonstrates a separation technique applicable to other acidic and basic drugs. It requires only extraction of the drug with methanol–water–acetic acid (66+33+1) and separation of insoluble material by filtration before HPLC. Labetalol, is chromatographically separated from soluble feed components by means of a µBondapak C18 column and methanol–water–acetic acid (66+33+1) mobile phase, 0.005M with respect to sodium dioctylsulfosuccinate pairedion reagent. Average recovery is 98.7% with a relative standard deviation of ±2.3% for the equipment described.

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