Current Issue : April - June Volume : 2016 Issue Number : 2 Articles : 8 Articles
Pharmaceutical testing laboratories operate under strict regulatory compliance and make important contributions to assuring quality of medicines provided. The testing is undertaken in a proper way and the results generated by them are accurate, reliable and reproducible. Adoption of ISO 17025 standard, which serves as a basis for laboratory accreditation, by the pharmaceutical laboratories would help to achieve these goals. Present article describes the various approaches which may be adopted by the pharmaceutical laboratories for assuring the quality of their test results. These approaches include: use of certified reference material and internal quality control, participation in inter-laboratory comparison and proficiency testing programs, replicate testing using the same or different methods, retesting of retained items and internal quality controls....
Andrographis paniculata is one of the most potent medicinal plants used in Indian traditional systems of medicine for the treatment of various diseases of mankind. The present study mainly aimed to estimate the content of major constituent andrographolide present in Andrographis paniculata collected from different regions of Tamilnadu and Kerala. HPTLC method was adopted for determining the content of the active constituent present in the plant using marker compound andrographolide. The HPTLC method was performed using HPTLC aluminium sheets precoated with silica gel 60 GF254 as stationary phase and ethyl acetate: n-hexane (8.5:1.5 v/v) as the mobile phase. The developed chromatogram was scanned at 233 nm using Camag scanner III. The Rf value of standard andrographolide and andrographolide in the aqueous leaf extract of Andrographis paniculata were found to be in the range of 0.28 to 0.33. The content of andrographolide was found to be high in leaves compared to other parts of the plant. Plant collected from Sirumalai hills, Dindigul, Tamilnadu and from Kuravilangad, Kerala was found to contain relatively high amount of marker compound andrographolide than other regions. Among these two regions the content of andrographolide was found to be high for the plants collected from Sirumalai hills, Dindigul region, Tamilnadu....
Cocculus hirsutus is a perennial climbing shrub having a broad spectrum activity against several ailments. Flavonoids present in a crude ethanolic extract of Cocculus hirsutus leaves were analysed. Rutin, liquirin and quercetin were used as calibration standards. Objective of this research was to develop and validate HPLC method for simultaneous determination of rutin, liquiritin and quercetin in Cocculus hirsutus leaves. The analysis was performed by reverse phase chromatography using Sil C-18 column (250 x 4.6 mm I. D., 10 μm particle size) as a stationary phase and methanol, water and 1 % acetic acid (40:60:2 v/v/v) as a mobile phase with an isocratic flow rate of 1 ml/min for 20 minutes and detection at a wavelength of 360 nm. Chromatographic conditions were optimized and results showed good peak resolution among rutin, liquitin and quercetin with retention time of 2.85, 3.79 and 15.44 min. respectively. Calibration curves were acquired with r2 > 0.997 and relative standard deviation values for intra- and inter-day precision were less than 2.0%. The recovery rate of each component in Cocculus hirsutus leaves in the range of 97.71 - 99.49 %. The contents of rutin, liquirin and quercetin in Cocculus hirsutus leaves were 48.11±0.03, 0.038±0.05 and 17.828±0.04%. Thus the proposed method was statically validated as per ICH guidelines. The proposed HPLC method can be implemented for simultaneous estimation of rutin, liquirin and quercetin in herbal medicinal plants and their products....
An oral fixed dose combination of netupitant as highly selective NK1 receptor antagonist and palonosetron as 5-HT3 receptor antagonist indicated for the prevention of chemotherapy induced nausea and vomiting (CINV). The shelf life of the product specifies the length of the period in which it remains fully effective under normal storage conditions and it was established by performing forced degradation studies. The current study was focussed to perform forced degradation studies for the combined capsule dosage form containing netupitant and palonosetron and to develop a stability indicating assay for the estimation of their potency simultaneously using isocratic RP-HPLC method with diode detection along with their degradation products. Optimized chromatographic conditions were established for the efficient separation and quantification of netupitant and palonosetron in the presence of their degradation products with excellent resolution and selectivity. The chromatographic separation of netupitant and palonosetron was achieved with a combination of an analytical C18 column (250 x 4.6 mm, 5m) as stationary phase, maintained at ambient temperature and mobile phase comprising of buffer and acetonitrile in the proportion of 62:38 (v/v) as mobile phase, pumped on to the column in isocratic mode at a flow rate of 1.0 ml/min. The eluents from the column were monitored at a wavelength of 254 nm using diode array detector and also performed peak purity analysis for detecting the co-eluting degradation products to ensure the accuracy of the quantification. Netupitant and palonosetron are subjected to acid, base, water, hydrogen peroxide, temperature, humidity and light to know the extent of degradation. The established method well separated the netupitant and palonosetron with their co-eluting peaks of degradation products with required resolution and selectivity and allowed to quantify simultaneously without any interference, demonstrating the stability indicating nature of the method. To know the stability indicating nature of the proposed RP-HPLC method, it was statistically validated as per international conference on harmonization (ICH) with respect to linearity, specificity, precision, accuracy and robustness, limit of detection and limit of quantification, including system suitability. The proposed method was found to be specific, selective, simple, rapid, economic, accurate and precise method and it could be suitable for routine laboratory analysis....
HPTLC method has been developed for determination of gallic acid and piperine in appetomax®, a polyherbal ayurvedic proprietary liquid oral formulation manufactured and marketed by Ocean Life care Pvt. Ltd., Pune, containing extracts form ten plant materials. Gallic acid (GA) and piperine (PI) are important compounds present in the formulation and were selected as marker analytes. Different volumes of sample were spotted for estimation of the GA (2 μl) and PI (40 μl) at 300 nm by densitometry using silica gel 60F254 as stationary phase. Mobile phase used consisted of toluene: methanol: acetic acid 8:1.5:0.5 (v/v/v), Rf values of GA and PI were 0.16±0.02 and 0.55±0.02 respectively. Linearity range was 80-280 ng/band and 60-260 ng/band and coefficient of determination was 0.996 and 0.992 for GA and PI respectively. Limits of detection and quantitation were recorded as 7 and 21 ng/band for GA and 6.67 and 20.21 ng/band for PI. The developed high performance thin layer chromatography method was validated for accuracy, precision, robustness, specificity as per ICH guidelines. Thus the methods can be used for the routine estimation of GA and PI in Ayurvedic proprietary liquid oral formulation....
Impurity profiling is the common name of a group of analytical activities, the aim of which is the detection, identification/structure elucidation and quantitative determination of organic and inorganic impurities, as well as residual solvents in bulk drugs and pharmaceutical formulations. The impurities present in the drug are adversely affecting the quality of the drug product. There are various types of impurities like starting materials, intermediates, penultimate impurity, by product and degradation product. Various regulatory authorities like ICH, USFDA, Canadian Drug and Health Agency are emphasizing on the purity requirements and the identification of impurities in Active Pharmaceutical Ingredient’s (API’s). Qualification of the impurities is the process of acquiring and evaluating data that establishes biological safety of an individual impurity; thus, revealing the need and scope of impurity profiling of drugs in pharmaceutical research. Identification of impurities is done by variety of Chromatographic and Spectroscopic techniques, either alone or in combination with other techniques. There are different methods for detecting and characterizing impurities with TLC, HPLC, HPTLC, AAS etc. Among all hyphenated techniques, the most exploited techniques, for impurity profiling of drugs are LC-MS-MS, LC-NMR, LCNMR-MS, GC-MS & LC-MS....
Validation is one of the important steps in achieving and maintaining the quality of the final product. If each step of production process is validated we can assure that the final product is of the best quality. Validation of the individual steps of the processes is called the process validation. Different dosage forms have different validation protocols. Here this article concentrates on the process validation of solid dosage forms, protocol preparation and regulatory basis for process validation with special emphasis on tablets in industry. Three consecutive batches of tablets shall be taken up for the validation process. It gives in detail the validation of each step of the manufacturing process....
An approach of forced degradation study was successfully applied for development and validation of stability indicating RRLC assay method for the simultaneous estimation and quantification of three anti-hypertensive drugs olmesartan medoxomil, hydrochlorothiazide and amlodipine besylate in marketed formulation in presence of its degradation products. The method showed separation of all three drugs from their associated degradation products. The separation was achieved on zorbax SB C18 column (50 x 4.6 mm id, 1.8 µm particle size) using mobile phase of triethylamine buffer solution (at pH 3): acetonitrile (gradient program). The flow rate was 1 ml/min, injection volume 3 µl and detection was done at 236 nm on photodiode array detector. Gradient program for RRLC method was used for proper separation of peaks. Comprehensive stress testing of all drugs was carried out as per ICH guideline Q1A (R2). There were no other coeluting, interfering peaks from excipients, impurities, or degradation products due to variable stress conditions and the method was specific for determination of all drugs in the presence of degradation products. The retention time for hydrochlorothiazide, amlodipine besylate and olmesartan medoxomil was 1.2 min, 1.8 min and 2.1 min respectively. The linearity of method was investigated in range of 5-40 µg/ml for olmesartan medoxomil, 3.125-25 µg/ml for hydrochlorothiazide and 1.25-10 µg/ml for amlodipine besylate respectively. Validation results showed satisfactory linearity, accuracy, precision, robustness and ruggedness. The detection wavelength of 236 nm was chosen in order to achieve a good sensitivity for quantitative determination of all drugs in solid dosage form. Method can be successfully employed for simultaneous estimation of all drugs in commercial products....
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