Stability Indicating RP-HPLC Estimation of Nebivolol Hydrochloride in Pharmaceutical Formulations

A simple, specific, accurate and stability indicating reversed phase liquid chromatographic method was developed for the determination of nebivolol hydrochloride in tablet dosage forms. A phenomenex Gemini C-18, 5 μm column having 250×4.6 mm i.d., with mobile phase containing methanol: acetonitrile: 0.02 M potassium dihydrogen phosphate (60:30:10, v/v/v; pH 4.0) was used. The retention time of nebivolol hydrochloride was 2.6 min. The linearity for nebivolol hydrochloride was in the range of 0.2-10 μg/ml. The recovery was found to be in the range of 98.68-100.86%. The detection limit and quantification limit were found to be 0.06 μg/ml and 0.2 μg/ml, respectively. Nebivolol stock solutions were subjected to acid, alkali and neutral hydrolysis, chemical oxidation and dry heat degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. The proposed method was validated and successfully applied to the estimation of nebivolol hydrochloride in tablet formulations.     

Development of a Validated Stability Indicating HPLC Method for Ranitidine Hydrochloride Syrup

An isocratic reversed-phase high-performance liquid chromatographic method was developed and validated for the determination of ranitidine HCl in syrup. The samples were analyzed by high-performance liquid chromatography (HPLC). Chromatographic separation was achieved on a C₁₈ column using an acetonitrile–aqueous phosphate buffer (20:80, v/v) elution, buffer being 10 mM disodium hydrogen phosphate brought to pH 7.1 with sodium hydroxide (0.1 N). Validation steps involved measurement of selectivity, accuracy, and precision under conditions of repeatability, reproducibility, sensitivity, and robustness. The lower limit of quantification was 10μg/mL. The validated method has been demonstrated to be reliable for the determination of ranitidine HCl and its related compound C. Stress degradation studies included exposing ranitidine HCl powder and Zantac syrup to acid, alkali, oxidation, and accelerated temperature of 50 °C for 24 hrs and photolysis for 8 hrs. The peaks of degraded products were well resolved from the drug peak. The validation of this method indicated that it could be effectively used to monitor the stability of ranitidine HCl syrup.     

New Stability Indicating RP-HPLC Method for the Estimation of Cefpirome Sulphate in Bulk and Pharmaceutical Dosage Forms

A simple stability indicating reversed-phase HPLC method was developed and subsequently validated for estimation of Cefpirome sulphate (CPS) present in pharmaceutical dosage forms. The proposed RP-HPLC method utilizes a LiChroCART-Lichrosphere100, C18 RP column (250 mm × 4mm × 5 μm) in an isocratic separation mode with mobile phase consisting of methanol and water in the proportion of 50:50 % (v/v), at a flow rate 1ml/min, and the effluent was monitored at 270 nm. The retention time of CPS was 2.733 min and its formulation was exposed to acidic, alkaline, photolytic, thermal and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. The described method was linear over a range of 0.5-200μg/ml. The percentage recovery was 99.46. F-test and t-test at 95% confidence level were used to check the intermediate precision data obtained under different experimental setups; the calculated value was found to be less than the critical value.     

Stability Indicating RP-HPLC Simultaneous Estimation of Hyoscine Butylbromide and Paracetamol in Tablets

Pharmaceutical Chemistry Journal - A stability indicating method was developed and validated for the quantitative simultaneous estimation of hyoscine butylbromide (HBB) and paracetamol (PAR) in a...     

A Validated RP-HPLC Method for Simultaneous Estimation of Nebivolol and Hydrochlorothiazide in Tablets

A simple, selective, rapid, precise and economical reverse phase high pressure liquid chromatographic method has been developed for the simultaneous estimation of nebivolol and hydrochlorthiazide from pharmaceutical formulation. Phenomenex Gemini C(18) (25 cm×4.6 mm i.d., 5 μ) column with a mobile phase consisting of acetonitrile: 50mM ammonium acetate (adjusted to pH 3.5 using orthophosphoric acid) (70:30 v/v) at a flow rate of 1.0 ml/min was used. Detection was carried out at 254 nm. Probenecid was used as an internal standard. The retention times of probenecid, nebivolol and hydrochlorthiazide were 13.05, 3.32 and 4.25 min, respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability. The proposed method can be used for the estimation of these drugs in combined dosage forms.     

Stability Indicating RP-HPLC Estimation of Atorvastatin Calcium and Amlodipine Besylate in Pharmaceutical Formulations

A simple, specific, accurate and stability indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of atorvastatin calcium and amlodipine besylate in tablet dosage forms. A phenomenex Gemini C-18, 5 μm column having 250×4.6 mm i.d. in isocratic mode, with mobile phase containing 0.02 M potassium dihydrogen phosphate:acetonitrile:methanol (30:10:60, v/v/v) adjusted to pH 4 using ortho phosphoric acid was used. The flow rate was 1.0 ml/min and effluents were monitored at 240 nm. The retention times of atorvastatin calcium and amlodipine besylate were 11.6 min and 4.5 min, respectively. The calibration curves were linear in the concentration range of 0.08-20 μg/ml for atorvastatin calcium and 0.1-20 μg/ml for amlodipine besylate. Atorvastatin calcium and amlodipine besylate stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. The proposed method was validated and successfully applied to the estimation of atorvastatin calcium and amlodipine besylate in combined tablet dosage forms.     

Stability Indicating RP-HPLC Method for Simultaneous Determination of Pholcodine and Guaiacol in Pharmaceutical Syrup

Pharmaceutical Chemistry Journal - Guaiacol (GUA) and pholcodine (PHO) were simultaneously determined in a pharmaceutical syrup using RP-HPLC with UV detection. The separation was performed using...     

Stability Indicating RP-HPLC Method for Simultaneous Determination of Simvastatin and Ezetimibe from Tablet Dosage Form

A simple, specific and sensitive reverse phase high performance liquid chromatographic method was developed and validated for simultaneous determination of ezetimibe and simvastatin from pharmaceutical dosage forms. The method uses C18 ODS Hypersil column and isocratic elution. The mobile phase composed of acetonitrile:phosphate buffer (pH 4.5, 0.01M) in the ratio of 65:35 v/v was used at a flow rate of 1.0 ml /min. UV detector was programmed at 232 nm for first 10 min and at 238 nm for 10 to 20 min. All the validation parameters were in acceptable range. The developed method was effectively applied to quantitate amount of ezetimibe and simvastatin from tablets. The method was also applied suitably for determining the degradation products of ezetimibe and simvastatin.     

Concurrent Estimation of Clopidogrel Bisulfate and Aspirin in Tablets by Validated RP-HPLC Method

A simple, rapid, precise RP-HPLC method was developed for simultaneous estimation of aspirin and clopidogrel bisulphate in tablet dosage form used in the treatment of cardiovascular diseases. To achieve the maximum resolution, acetonitrile:50 mM potassium dihydrogen phosphate buffer:methanol, solution pH adjusted to 3, in the ratio 50:30:20; v/v was selected as mobile phase. This mixture was found to be appropriate allowing good separation of both the components at a flow rate of 1.5 ml/min and detection wavelength 240 nm. In these conditions clopidogrel bisulfate and aspirin were eluated at the 7.47 and 2.2 min. The linearity was found in the concentration range 1.5-7.5 and 3.5-15.0 μg/ml, respectively. All the analytical validation parameters were determined and found with in the limit as per ICH guideline, which indicates the validity of method.     

黄芩苷水溶液的稳定性

目的采用RP-HPLC法考察了黄芩苷水溶液的稳定性.方法采用经典恒温加速试验考察了温度对黄芩苷水溶液的影响,并测定了黄芩苷水溶液的最稳定pH.结果黄芩苷水溶液损失10%所需要的时间仅为18.1 h,降解活化能为79.1kJ·moL-1.黄芩苷的最稳定pH值采用实测值为4.28.结论黄芩苷水溶液受温度和pH的影响很大,因此在生产过程中,应尽可能保持低温,并调节溶液pH值使接近黄芩苷的最稳定pH.     

A Stability Indicating Method for the Determination of the Antioxidant Sodium Bisulfite in Pharmaceutical Formulation by RP-HPLC Technique

A stability-indicating reversed-phase high-performance liquid chromatographic (RP-HPLC) method was developed for the determination of sodium bisulfate (SB), an antioxidant, in injectable dosage form. The chromatographic separation was achieved on a Zorbax CN (250 mm × 4.6 mm, 5 μm) column, with a mobile phase consisting of a buffer mixture of 0.03 M tetrabutylammonium hydrogen sulfate, 0.01 M potassium dihydrogen orthophosphate, and acetonitrile at a ratio of 70:30 (v/v) and a flow rate of 0.7 mL/min. The eluted compound was monitored at a wavelength of 215 nm using a UV detector. The method described herein separated sodium bisulfite from all other formulation components within a run time of 10 min. The method also generated linear results over an SB concentration range of 10 to 990 μg/mL, and the limit of quantification was found to be 10 μg/mL. The stability indicating capability of the method was established by performing forced degradation experiments. The RP-HPLC method that was developed was validated according to the International Conference on Harmonization (ICH) guidelines. This method was successfully applied in the quantitative determination of SB in a stability study of Amikacin sulfate injection. The procedure described herein is simple, selective, and reliable for routine quality control analysis as well as stability testing.     

A Validated RP-HPLC Method for the Estimation of Lapatinib in Tablet Dosage form using Gemcitabine Hydrochloride as an Internal Standard

A simple, selective, rapid, precise and economical reverse-phase high-performance liquid chromatography method has been developed for the determination of lapatinib in tablet using gemcitabine hydrochloride as an internal standard. Chromatography was carried out on an ODS C-18 RP column (4.6 mm i.d. ×250 mm) using a mixture of acetonitrile and water (50:50 v/v) as the mobile phase at a flow rate of 1.0 ml/min. The drug was monitored at 232 nm. The retention times for lapatinib and gemcitabine hydrochloride were found to be 4.25±0.05 and 6.10±0.05 min, respectively. The method produced linear responses in the concentration range of 2-60 μg/ml of lapatinib. The limit of detection and limit of quantitation were 0.265 and 0.884 μg/ml, respectively.     

Validated Stability-Indicating RP-HPLC Method for the Estimation of Degradation Behaviour of Organic Peroxide and Third-Generation Synthetic Retinoids in Topical Pharmaceutical Dosage Formulation

The objective of the current study was to establish a validated stability-indicating, high-performance liquid chromatographic method to determine the purity of benzoyl peroxide (BPO) and adapalene (ADP) in the presence of its impurities, forced degradation products, and placebo in pharmaceutical dosage forms. The desired chromatographic separation was achieved on the Kinetex^™ C18 (250 × 4.6 mm, 5 µm) column using gradient elution at 272 nm detection wavelength. The optimized mobile phase consisted of solvent A (mixture of 0.1% v/v glacial acetic acid in water and acetonitrile in the ratio of 80:20 v/v, respectively) and solvent B (mixture of acetonitrile: tetrahydrofuran: methanol in the ratio of 50:30:20 v/v/v, respectively). The stability-indicating capability of the developed method was established by analysing forced degradation samples in which the spectral purity of BPO and ADP along with separation of all degradation products from the analyte peaks was achieved. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision, and robustness.     

Validated LC Method for the Estimation of Voriconazole in Bulk and Formulation

Reversed phase high performance liquid chromatographic method was developed and validated for the estimation of voriconazole in bulk and formulation using prominence diode array detector. Selected mobile phase was a combination of water:acetonitrile (35:65 % v/v) and wavelength selected was 256 nm. Retention time of voriconazole was 3.95 min. Linearity of the method was found to be 0.1 to 2 μg/ml, with the regression coefficient of 0.999. This method was validated according to ICH guidelines. Quantification was done by calculating area of the peak and the detection limit and quantitation limit ware 0.026 μg/ml and 0.1 μg/ml, respectively. There was no significant difference in the intra day and inter day analysis of voriconazole determined for three different concentrations using this method. Present method can be applied for the determination of voriconazole in quality control of formulation without interference of the excipients.     

Stability Indicating HPLC Method for Simultaneous Determination of Mephenesin and Diclofenac Diethylamine

A simple, specific, accurate and stability-indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of mephenesin and diclofenac diethylamine, using a Spheri-5-RP-18 column and a mobile phase composed of methanol: water (70:30, v/v), pH 3.0 adjusted with o-phosphoric acid. The retention times of mephenesin and diclofenac diethylamine were found to be 3.9 min and 14.5 min, respectively. Linearity was established for mephenesin and diclofenac diethylamine in the range of 50-300 μg/ml and 10-60 μg/ml, respectively. The percentage recoveries of mephenesin and diclofenac diethylamine were found to be in the range of 99.06-100.60% and 98.95-99.98%, respectively. Both the drugs were subjected to acid, alkali and neutral hydrolysis, oxidation, dry heat, photolytic and UV degradation. The degradation studies indicated, mephenesin to be susceptible to neutral hydrolysis, while diclofenac diethylamine showed degradation in acid, H₂O₂, photolytic and in presence of UV radiation. The degradation products of diclofenac diethylamine in acidic and photolytic conditions were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for simultaneous quantitative analysis of mephenesin and diclofenac diethylamine in bulk drugs and formulations.     

A New Stability Indicating HPLC Method for Related Substances in Zolmitriptan

A sensitive, precise, specific, linear and stability indicating isocratic HPLC method was developed for the analysis of related substances in zolmitriptan. The potential known related substances are (S)-4-(4-aminobenzyl)-1,3-oxazolidin-2-one (impurity I) and (S)-4-(4-hydrazinobenzyl)-1,3-oxazolidin-2-one (impurity II). The method can be used for the detection and quantification of known and unknown impurities and degradants in the drug substance zolmitriptan during routine analysis and also for stability studies in view of its capability to separate degradation products.     

Validated RP-HPLC Method for Simultaneous Quantitation of Losartan Potassium and Metolazone in Bulk Drug and Formulation

A HPLC method has been described for simultaneous determination of Losartan potassium and Metolazone in formulation. This method is based on a HPLC separation of the two drugs on the Thermo Hypersil BDS-C(18) (250 mm × 4.6 mm, 5.0 μm) with isocratic conditions and a simple mobile phase containing acetonitrile:water (60:40) at a flow rate of 0.8 mL/min using UV detection at 237 nm. This method has been applied to a marketed formulation without interference of excipients. The linear regression analysis data for the calibration plots showed a good linear relationship over the concentration range of 2-12 μg/mL for Losartan potassium and 0.2-1.2 μg/mL for Metolazone, respectively. The method was validated for precision, robustness and recovery. Statistical analysis showed that the method is repeatable and selective for the estimation of Losartan potassium and Metolazone.     

Validated RP-HPLC Method Development for Gentamicin Microanalysis in Pharmaceutical Dosage Forms,Urine and Blood

Pharmaceutical Chemistry Journal - Gentamicin is an important member of the aminoglycoside class of antibiotics having broader spectrum with extend to ototoxicity and nephrotoxcity. A reliable and...     

Stability-Indicating RP-HPLC Method for Estimation of Miglitol in Bulk and Tablets

A selective and sensitive, stability-indicating reverse phase high performance liquid chromatography method has been first developed and validated for the estimation of miglitol in bulk and tablet dosages form. Samples were separated on a prepacked, Inertsil amino C(18) column (150×4.6 mm i.d.) using a mobile phase comprised of acetonitrile and monobasic sodium phosphate pH 7.5 (80:20, v/v) delivered at 1.5 ml/min flow rate. Detection was performed on a SPD-20A prominence UV/Vis detector at 220 nm. The retention time for miglitol was 13.93±0.0367. The method was validated in terms of linearity, precision, accuracy, ruggedness, and specificity, limit of detection and limit of quantification. The linearity (r(2)) and percentage recoveries of miglitol were 0.9986 and 99.85%. This method is suitable for routine estimation of miglitol in bulk and tablet dosages form.