ABSTRACT
A simple, accurate, precise and robust stability indicating RP-HPLC assay method has been developed for the estimation of trimethobenzamide in stress sample. An isocratic separation of trimethobenzamide was achieved on Kromasil 100 C-18 column (250 X 4.6mm, 5µ) with a flow rate of 1.0 ml/min and by using a photodiode array detector to detect the analyte at 213nm. The optimized mobile phase consisted of methanol: ammonium formate (44:56, v/v). The drug was subjected to different forced degradation conditions according to ICH guidelines including acid, base, neutral hydrolysis, oxidation, photolysis and thermal degradation. Degradation products were found only in basic and oxidative degradation conditions. All the degradation products got eluted in an overall analytical run time of 12min. The developed analytical method has been validated according to the ICH guidelines. Response of trimethobenzamide was linear over the concentration range of 0.5-50µg/mL (r2 = 0.999). Accuracy was found to be in between 94.03% to 100.39%. Degradation products resulting from the stress studies did not interfere with the detection of the analyte.
Subject(s)
Chromatography, High Pressure Liquid/methods , /analysis , Validation Study , Methods , Pharmaceutical Preparations/administration & dosage , HydrolysisABSTRACT
A simple, rapid, precise, accurate and sensitive spectrophotometric method has been developed for the simultaneous estimation and validation of Nebivolol Hydrochloride (NEB) and Valsartan (VAL) in pure and combined tablet dosage forms. Pure drug samples of NEB and VAL were dissolved in 67 mM Phosphate buffer pH 6.8 with 0.5 % sodium dodecyl sulphate (SDS) and found to have absorbance maxima at 280 nm for NEB and 250 nm for VAL, respectively. The linearity lies between 10-70 μg/ml for NEB and 10-60 μg/ml for VAL in this method. The correlation coefficient (r2) was found to be 0.9965 for NEB and 0.9960 for VAL. The % recoveries obtained were 95.65 % – 109.85 % for NEB and 97.42 % – 101.43 % for VAL. The % RSD found 0.271 %-1.490 % for intraday and 0.334 %-1.917 % for interday for NEB and 0.188 %-0.944 % for intraday and 0.392 %-1.197 % for interday for VAL. The limit of detection and limit of quantitation for NEB were found to be 4.608 μg/ml and 13.965 μg/ml respectively and the limit of detection and limit of quantitation for VAL were found to be 4.348 μg/ml and 13.178 μg/ml respectively. Simultaneous calibration of both drugs in 67 mM Phosphate buffer pH 6.8 with 0.5 % SDS shows that λmax of one drug does not interfere on the λmax of other drug. Recovery study was performed to confirm the accuracy of the method. The results of analysis have been validated statistically by recovery studies as per International Conference on Harmonization guidelines. The method showed good reproducibility and recovery with % RSD <2. Hence, this proposed method was found to be rapid, specific, precise, accurate and can be successfully applied for the routine analysis of NEB and VAL in pure and combined tablet dosage form.
ABSTRACT
A simple, accurate, isocratic stability indicating RP-HPLC method was developed for the determination of cefepime and amikacin in Pure and its pharmaceutical formulations. The method consists of methanol: acetonitrile:acetate buffer 75:20:05 (v/v) mobile phase at pH 5.1 with C18 column as stationary phase. The flow rate and detection wave length were 1.0 mL/min and 212 nm respectively. The linearity range for the method was found to be 2.5-25 µg/mL for amikacin and 10-100 µg/mL cefepime respectively. The developed method was validated as per ICH guidelines and the results of all the validation parameters were well within their acceptance values. Also the forced degradation studies were conducted with standard drugs. Degradation products formed during the different stress conditions were separated from both drugs. This validated method was applied for the simultaneous estimation of cefepime and amikacin in commercially available formulation sample.
Subject(s)
Amikacin/analysis , Chromatography, High Pressure Liquid/methods , Validation Study , Pharmaceutical PreparationsABSTRACT
A simple, highly sensitive stability indicating reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed and validated for the determination of sumatriptan succinate in bulk and tablet dosage form. The analysis was performed on reverse phase C18 ODS Inertsil (250×4.6mm, 5μm) column, with a mobile phase containing buffer: aetonitrile: methanol (80:10:10 v/v/v), pH was adjusted to 2.5 with orthophosphoric acid (OPA) at 221nm, by an isocratic elution mode with 1ml/min flow rate using photo diode array (PDA) detector at ambient temperature. The injection volume and retention time was found 20 μl and 4.4 minutes respectively. The method produced linear responses in the concentration range of 5-150 μg/ml, with a correlation coefficient of 0.999. The limit of detection (LOD) and limit of quantification (LOQ) values for HPLC method were found to be 1.967 and 5.961 μg/ml respectively. The recovery of the method was 98% of the labelled value. This method was validated for accuracy, precision, linearity and robustness. Sumatriptan subjected to different ICH prescribed stress conditions of acid, alkali, peroxide, reduction, thermal, photolytic and humidity degradation. This method can easily and conveniently take up for routine quantitative analysis of sumatriptan in bulk and pharmaceutical dosage form by easily available materials with low cost.
ABSTRACT
A simple, rapid and precise reverse phase liquid chromatographic (RP-HPLC) method was developed and subsequently validated for simultaneous estimation of Cefpodoxime proxetil and Ofloxacin in combined fixed dose oral formulation. The analysis was carried out using X-terra C8 (4.6 x 250mm, 5μm, Make: ACE), prepacked column. The separation was carried out using a mobile phase containing a 0.25%v/v triethyl amine buffer of pH 3.5 and acetonitrile (30:70 v/v), was pumped at a flow rate of 1.2 ml/min with UV-detector and PDA detection at 227 nm. Both the drugs were well resolved on the stationary phase and the retention times were around 2.747 minute for Cefpodoxime proxetil and 2.076 minute for Ofloxacin. The method was validated and shown to be linear for Cefpodoxime proxetil and Ofloxacin. The correlation coefficients for Cefpodoxime proxetil and Ofloxacin are 0.998 and 0.999 respectively. The relative standard deviations for five replicate measurements in two sets of each drug in the tablets is always less than 2% and mean % error of active recovery not more than ±1.5%. The method was validated for precision and accuracy. The developed method could be applied for routine analysis of Cefpodoxime proxetil and Ofloxacin in tablet dosage form without any interference of excipients.
ABSTRACT
A reverse phase high performance liquid chromatographic method was developed for the determination of dulox-etine hydrochloride in bulk and dosage form. The separation was effected on a kromasil ODS C18 column (250mmX4.6mm, 5μ) using a mobile phase mixture of buffer and methanol in a ratio of 85:15 v/v at a flow rate of 1.0ml/min. The detection was made at 230nm. The retention time of duloxetine hydrochloride was found to be 3.443±0.06 min. Calibration curve was linear over the concentration range of 20-120μg/ml of duloxetine hydrochlo-ride. The propose method was validated as per the ICH guidelines. The method was accurate, precise, specific and rapid found to be suitable for the quantitative analysis of the drug and dosage form.
ABSTRACT
A reverse phase high performance liquid chromatographic method was developed for the determination of dulox-etine hydrochloride in bulk and dosage form. The separation was effected on a kromasil ODS C18 column (250mmX4.6mm, 5μ) using a mobile phase mixture of buffer and methanol in a ratio of 85:15 v/v at a flow rate of 1.0ml/min. The detection was made at 230nm. The retention time of duloxetine hydrochloride was found to be 3.443±0.06 min. Calibration curve was linear over the concentration range of 20-120μg/ml of duloxetine hydrochlo-ride. The propose method was validated as per the ICH guidelines. The method was accurate, precise, specific and rapid found to be suitable for the quantitative analysis of the drug and dosage form.