Current Issue : April - June Volume : 2015 Issue Number : 2 Articles : 8 Articles
A sensitive, precise, specific, linear and stability-indicating high performance thin-layer chromatographic (HPTLC) method has been established and validated for quantitative analysis of one of the antidiabetic agents, the sulfonylurease glipizide in active pharmaceutical ingredient (API) and in tablet formulation, using toluene: methanol (8:2; v/v) as mobile phase. Chromatographic separation was achieved on precoated silica gel 60F254 plates with 0.2 mm thickness. Detection and quantification were performed by classical densitometry using a UV detector at 230 nm. Compact spots were obtained for glipizide (RF 0.35±0.02, mean±SD). Calibration plots were constructed in the range 100-700 ng per band and were linear with good calibration coefficients (r = 0.9997±0.01, mean±SD) for glipizide. The limit of detection and quantification were 100 and 300 ng per spot for glipizide. Glipizide was subjected to the international conference on harmonization (ICH) prescribed hydrolytic (acid, base and neutral), oxidative, photolytic and thermal stress conditions. Among all the above mentioned conditions, the drug was found to be susceptible to some stress conditions. However, the degradation products were well resolved from the pure drugs with significantly different RF values....
The simple, accurate, precise, reproducible and economic UV spectroscopic methods of quinine and ciprofloxacin have been developed for the simultaneous estimation. The method A-dual wavelength, method B-area under curve and method C-absorption ratio method were developed by using JASCO double beam UV Spectrophotometer (model-V630). As simultaneous estimation was carried out, measurement of absorbance at two wavelengths 233 nm and 272 nm which shows λmax values of quinine and ciprofloxacin respectively in distilled water. Quinine and ciprofloxacin shows linearity at selected wavelengths and obeys beers law in the concentration range of 5-30 µg/ml with good correlation coefficient 0.998 and 0.991 respectively. For the area under curve the wavelength selected for quinine was from 227 nm to 237 nm and for ciprofloxacin 264 nm to 279 nm which gives peak area for quinine 0.370041 and for ciprofloxacin 3.60596. For the method C involved formation of isoabsorptive point at 246 nm....
Five simple and cost-conscious UV spectrophotometric methods (A-E) has been developed and validated for the\ndetermination of avitriptan in bulk and pharmaceutical formulations. These methods were based on the formulation of colored\ncomplex of avitriptan with different reagents. The absorbance of the formed color complex was measured at the wavelength of\nmaximum absorbance of the complex against the reagent blank. Method A and B were based on the formation of colored species\nbetween the avitriptan and TPooo and ARS by means of ion association complex formation reaction. The absorbance was\nmeasured at max = 560 for method A and max = 590 for method B. Method C was based on the reaction of avitriptan with folin to\nform a blue colored species having absorption maxima at max = 450 nm. Method D was based on the formation of diazotization\ncoupling of drug with PNA a colored species was found and exhibit absorption maxima at max = 470 nm. Method E was based on\noxidation followed by complex formation with 2,2�- bipyridyl in the presence of ferric chloride having absorption maxima at max\n= 400 nm. All these methods have different linearity ranges. Statistical analysis proves that the proposed methods were\nreproducible and selective for the estimation of avitriptan in bulk drug and in its tablet dosage form....
A reversed phase high performance liquid chromatography method (HPLC) coupled with a diode array; UV spectrometer was developed for the quantitative and qualitative standardization of salicin from Salix alba L. Salicin were separated on an phenomenox C18 column (250 mm × 4.6 mm I.D., 5µm), with a mobile phase composed of 0.1 % ortho-phosphoric acid (OPA) in water and acetonitrile, under gradient elution. The method was shown to be linear (r2 > 0.99), repeatable with instrumental precision < 2.0 and intra-assay precision < 2.0 (% CV, percent coefficient of variation), precise with intra-day variation < 2.0 and inter-day variation < 2.0 (% CV, percent coefficient of variation) and sensitive over the calibration range for salicin. Salicin is fully recovered in the presence of normal condition (recovery rates > 95%). Statistical analysis proves that the proposed method was more accurate, selective, reproducible and repeatable for the estimation of the salicin from Salix alba....
A new, simple, sensitive, selective, precise and robust reverse phase high pressure liquid chromatographic (HPLC) method was developed and validated for the determination of meloxicam (ME) and thiocolchicoside (THIO) in tablet and other pharmaceutical dosage forms. Analysis was carried out on Shimadzu HPLC system with kromasil C18 column (180 x 4.6 mm i.d, 5 μm particle size) using isocratic mode of methanol: acetonitrile: 0.1% v/v hexane sulfonic acid in HPLC grade water (15:10:65) as mobile phase with flow rate of 0.9 ml min-1. The detection was carried out using UV detector set at 254 nm by an injection volume of 20 μl and entire separation was carried out at 35°C column temperature. For this method, Beer’s law is obeyed in the concentration range of 4.0 to 20.0 μg ml–1 of meloxicam and 2.0 to 10.0 μg ml–1 of thiocolchicoside having linear regression equation of R-values of 0.994 and 0.996 respectively. The mean percent recoveries were found to be in the ranges of 100.43% - 101.67% for meloxicam and 99.00% - 101.62% for thiocolchicoside. The developed method has been successfully applied for the analysis of both the drugs in bulk and pharmaceutical formulations. The method was validated as per ICH guidelines by determining its specificity, accuracy, precision, linearity and range, ruggedness, robustness and system suitability....
Tenofovir disoproxil fumarate is an antiretroviral drug. In the present work, a simple, sensitive, specific method has been developed for the quantitative estimation of tenofovir disoproxil fumarate in bulk and pharmaceutical dosage form. Tenofovir disoproxil fumarate reacts with NQS reagent produce a colour complex which shows absorption maxima at 453 nm. The linearity was found in concentration range of 20-100 μg/ml. The correlation coefficient was found to be 0.9915. The method was validated as per ICH guidelines....
A simple, precise and economic high-performance liquid chromatographic method was developed for estimation of\nclotrimazole in commercial semisolid formulations. Metronidazole was used as internal standard. The retention time of\nclotrimazole and metronidazole was 10.6 min and 3.2 min respectively. Calibration curve was linear in the range of 10-50\n�¼g/ml. The values of RSD determined for precision, accuracy and robustness studies were less than 2%. The limits of detection\nand quantification were found to be 1 �¼g/ml and 3 �¼g/ml respectively. The proposed validated method can be employed for\nroutine quality control analysis of vaginal formulations as per international conference on harmonization guidelines....
A simple, rapid, accurate, precise and economic spectrophotometric method was developed for determination of p-coumaric acid in Cynodon dactylon Linn. In this method p-Coumaric acid shows absorbance maximum at different wavelength in different solvents, so absorbance was measured and the same wavelengths used for the estimation of p-Coumaric acid in respective solvents. p-Coumaric acid obeys the beer lamberts’ law. Method was validated according to ICH guideline and carried out for analysis of p-Coumaric acid....
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