Current Issue : January-March Volume : 2017 Issue Number : 1 Articles : 7 Articles
ICH Q3D recommends that manufacturers conduct a product risk assessment by first identifying known and potential sources of elemental impurities. Manufacturers should consider all potential sources of elemental impurities, such as elements intentionally added, elements potentially present in the materials used to prepare the drug product, and elements potentially introduced from manufacturing equipment or container closure systems. Manufacturers should then evaluate each elemental impurity likely to be present in the drug product by determining the observed or predicted level of the impurity and comparing it with the established PDE. The present study is a practical approach to control elemental impurities where potential sources of elemental impurities identified based on the declarations from suppliers. In this study, five elements (cadmium, lead, cobalt, vanadium, and nickel) were determined by axial view inductively coupled plasma optical emission spectrometry in drug substance atazanavir and cobicistat. The RF power was used 1150 watts, nebulizer gas flow was used 0.50 mL/min, auxillary flow was kept at 12 L/min, and flush pump rate was kept at 100 rpm. Nitric acid in water is used as diluent. Specifically, three representative production scale batches of drug substance atazanavir and cobicistat were tested and the results were within the acceptance criteria as per ICH Q3D....
There are only few published reports on determination of residual solvents in the analytical method development and there exists no detailed guidelines. Residual solvents from the process in the manufacturing of pharmaceuticals are hazardous and cause serious problems, so must be removed. This work is focused on the determination of analytical method for the determination of residual solvents. Bendamustine hydrochloride pure drug, various solvents, Shimadzu GC-2010 with head space auto injector and AOC ââ?¬â?? 5000 with head space auto injector were used. The method development based on residual solvent properties and many trails conducted on conditions like column selection, carrier gas flow, oven temperature and diluent. A simple HS-GC method for the determination of residual solvents in bendamustine hydrochloride using helium as the carrier gas at 3.0 ml/min with DB-624 (30.0 meters X 0.53 mm ID, 3.0Ã?µm d.f. capillary) as column using FID as detector was developed. The developed method was validated and parameters were to be found within the limits of USP. The retention time for residual solvents individually and in spiked standard solution was determined. The %RSD for six injections should be NMT15%. The percentage recovery ranges from 84.57-118.86%. The correlation coefficient was R2 ââ?°Â¥ 0.999. The method was validated for repeatability, linearity, limit of detection, limit of quantification and recovery according to the International Conference on Harmonization guidelines. The method validation results indicate that the method was accurate, precise, linear and sensitive for solvents assessed. Excellent results were obtained, within the globally accepted validation reference values, particularly taking into account the low concentration levels investigated....
A reverse phase high performance liquid chromatography (RP-HPLC) method was developed for estimation of artesunate without the use of buffer solution in mobile phase. Isocratic elution was achieved by use of acetonitrile: methanol: water as mobile phase. A C18 column of dimension 250 mm x 4.6 mm, 5 �µ was used and the flow rate was maintained at 1.2 ml/min. Artesunate was detected using UV detector at 220 nm. The linearity was evaluated between concentrations 800 to 4000 �µg/ml. The method was validated further for specificity, accuracy and precision. Artesunate was subjected to acid hydrolysis, base hydrolysis and oxidation for carrying out forced degradation studies....
The aim of present investigation was to develop dissolution method for evaluation of metoclopramide tablet. Different dissolution condition such as type of USP apparatus, speed of rotation of paddle and pH of dissolution medium were evaluated. The best in-vitro conditions obtained with phosphate buffer having pH 6.8 as a dissolution medium, USP Type II apparatus and 50 rpm speed were found to be most satisfactory. The release of drug analysed by using UV-visible spectrophotometric method which had regression coefficient 0.999 at concentration range 5-25 ppm. The dissolution test developed was adequate for its longer discriminative capacity in the release characteristic of product and could be applied for in-vitro evaluation of metoclopramide tablet....
For estimation of metoclopramide in pharmaceutical dosage form, a simple, accurate and precise area under curve spectrophotometric method was developed. ââ?¬Å?The area under two points on the mixture spectra is directly proportional to the concentration of the component of interestââ?¬Â is the AUC curve. The area selected for estimation of metoclopramide was between 262 to 282 nm. The method represented regression coefficient (r2= 0.999) at concentration rang 5-25 Ã?µg/ml. Estimation of the drugs was found upto 100 % representing the accuracy of the method. The recovery of the metoclopramide was found upto 100 %. Validation of the proposed method was carried out for its accuracy, precision and specificity according to ICH Q2 (R1) guidelines. The developed methods can be successfully applied in routine work for the estimation of metoclopramide in its pharmaceutical dosage form.Ã?©Ã?²...
The aim of present work was to develop an accurate, simple and cost effective UV spectrophotometric method for estimation of Teneligliptine. This method was based on area under curve of UV spectrum between 235-255nm and validation as per ICH guideline Q2 (R1). The method has followed linearity in the range of 10-50 �¼g /ml. The value of correlation coefficient was 0.9981 satisfactory value of percent relative standard deviation for the intraday and inter-day precision indicates that method was precise. Result of the recovery studies (99.25) shows accuracy of method. The developed method can be used for routine estimation of teneligliptine in bulk and dosage form....
A simple, accurate, precise and sensitive reverse phase liquid chromatography (RP-HPLC) methods was developed and validated for simultaneous estimation of chlorthalidone (CLT) and olmesartan medoxomil (OLM) in tablet dosage form using a Enable C18 (250 mm, -4.6 mm, 5 �¼m particle size) column and methanol: acetonitrile: water (60:20:20 v/v) as a mobile phase at a flow rate of 1.0 ml/min with detection wavelength 220 nm. The retention time for OLM and CLT was obtained as 1.89�±0.1 min and 2.98�±0.2 min respectively. The linearity was found in the range of 6.25-37.50 �¼g/ml and 10-60 �¼g/ml for CLT and OLM respectively. The developed method was validated as per ICH guideline, for its accuracy, precision, limit of detection and limit of quantitation....
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