Current Issue : July - September Volume : 2010 Issue Number : 2 Articles : 12 Articles
Column chromatography and proton nuclear magnetic resonance (1H NMR) spectroscopy were used to set up a new analytical method to determine the composition of aliphatic alcohols and steroidal alcohols, namely 4-desmethylsterols, 4-monomethylsterols and 4,4’-dimethylsterols, of an olive oil sample. Aliphatic and steroidal alcohols are the minor components of the oil unsaponifiable fraction obtained generally by solvent extraction after oil alkaline hydrolysis with a potassium hydroxide solution. The new analytical method applied column chromatography to separate triacylglycerols from polar components ruling out any chemical reaction on the oil sample. Moreover, the use of 1HNMR spectroscopy , with a low resolution power but with a high sensitivity as compared to 13C NMR, enabled the selection of diagnostic resonances of the 1H spectrum of minor components isolated as a mixture from CC. Composition of aliphatic alcohols (only long chain alcohols), of -sitosterol (a 4-desmethylsterol), of citrostadienol (a 4-monomethylsterol), of 24-methylenecycloartanol and cycloartenol (4,4’-dimethylsterols), of triacylglycerols, and of 1,2- and 1,3-diacylglycerols, could be determined....
Stability is defined as the capacity of a drug substance or drug product to remain within the established specifications to maintain its identity, strength, quality and purity through out the retest or expiration dating period. Any physical, chemical or microbiological change in the product potentially impact the efficiency and integrity of the final product and may therefore directly or indirectly impact patients’ health. To investigate potential stability issues of the drug in muzox tablet, accelerated and intermediated stability studies were carried out according to ICH guidelines at 300C+20C/65%RH+ 5%RH and 400C+20C/75%RH+5%RH for six month. Stability studies were carried out using programmable environmental test chamber CHM-10s, serial no. ICH-2530 and ICH 2531 (remi instrument ltd, Mumbai) and assay was carried out by using HPLC (Jasco) method which has been developed previously. The stability testing of muzox tablets showed there was no significance change in the content of Tramadol hydrochloride and Chlorzoxazone after 6 month of storage under controlled of temperature and humidity, at 300C+20C/65%RH+5%RH. Accelerated conditions under 400C+20C/75%RH+5%RH, dosage forms exhibit slight but insignificant fall within assay value. The parameters such as appearance, hardness, friability, disintegration time periods were determined at regular interval of each month for total period of six months. It showed that there was no change in physical parameter for six months at stored condition. Periods for electrical cut off and other related problems were compensated by extending the study for the relevant periods....
Simple , sensitive and accurate derivative and derivative ratio spectrophotometric methods are developed for quantitative estimation of each of cefprozil monohydrate (CZ) , cephapirin sodium (CN) and cefepime hydrochloride (CM), both in mixture with their alkaline degradation products (DCZ1, DCZ2 , DCN or DCM), respectively, and in their pharmaceutical dosage forms. A derivative ratio spectrophotometric method is designed for the simultaneous determination of either (CZ) or (CN) and (DCZ1 or DCN), respectively. For CZ the method involves measurements at 315 and peak-trough at 280-315 nm for CZ and at 331.8 nm for DCZ1. Meanwhile (CN) and (DCN) were quantitatively estimated in ethanol: water (1:1) solvent mixture by measurements at 239.2 and 238 nm, respectively. Moreover, DCN in mixture could be also assayed by recording the second derivative ratio spectra at 333 nm. Another derivative ratio spectrophotometric method permits the determination of either (CZ) or (CM) in presence of (DCZ2 or DCM), respectively, in water. (CZ) is measured at 318.4 nm while (CM) is measured at 250 or 285 and peak-trough at 250-285 nm. In addition first derivative spectrophotometric technique allows the simultaneous quantitative estimation of (CN) and (DCN) at 244 and 345 nm, respectively, in water: ethanol (1:1) mixture. Meanwhile, (DCN) is also successfully quantitated by measuring its absorbance in the zero-order spectrum at 330 nm. Statistical comparison of the results with reference methods indicate no significant differences in accuracy and precision....
A simple, sensitive, accurate, rapid and economical spectrophotometric methods have been developed and validated for the estimation of metronidazole (MET) and ofloxacin (OFX) in pH 6.8 phosphate buffer (simulated intestinal fluid, SIF). The drugs were estimated from the bulk and pharmaceutical dosage forms. The max were found to be 321 and 288 nm for MET and OFX respectively alone and in combination. The proposed methods have permitted the quantification of MET and OFX over linearity in the range of 0.5-20 and 5-50 g/mL for their individual and simultaneous estimation respectively. The methods were validated as per USP and ICH guidelines for the parameters such as recovery, precision, ruggedness and repeatability. The low RSD values of less than 1.14% indicated that the proposed methods were accurate. The RSD values for intra-day and inter-day variation were obtained between 0.49-1.38% and 0.34-1.59% respectively. The estimated drugs from the formulations containing MET and OFX alone were between 396.1(±3.81) to 403.5(±2.96)mg and 198.9(±2.64) to 203.66(±1.83)mg respectively. Further the drug concentrations in the formulations containing MET and OFX in combination were between 198.69(±2.72) to 202.59(±1.55)mg respectively. The low RSD value of less than 1.37% indicate that drugs from marketed tablet formulations can be analyzed using the proposed methods. The methods could be aimed at estimating MET and OFX in SIF containing pH 6.8 phosphate buffer for regular quality control testing....
A simple, accurate and precise validated RP-HPLC method for determination of Sirolimus has been developed. Analysis was carried out on Shimadzu HPLC system with Kromasil C18 column (180 x 4.6 mm i.d, 5µm particle size) using Acetonitrile: 0.01 % v/v Ortho-phosphoric acid in gradient proportion (Analysis time 0 min, 50% acetonitrile; analysis time 15 min, 75% acetonitrile; analysis time 15.1 min, 50% acetonitrile; analysis time 20 min, 50% acetonitrile) as mobile phase with flow rate of 1.3 mLmin-1. The detection was carried out using UV detector set at 277 nm. For this method, Beer’s law is obeyed in the concentration range of 20.0 to 80.0 µg mL–1 of Sirolimus. The developed method has been successfully applied for the analysis of drug in bulk and pharmaceutical formulations. The mean percent recoveries were found to be 98.8 ± 0.5 for Brand formulation. The method was validated with respect to linearity, precision and accuracy as per the International Conference on Harmonisation (ICH) guidelines....
A simple, rapid, precise and accurate reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of nateglinide in combination with metformin. This method uses an ODSA C18 analytical column, a mobile phase acetonitrile and buffer containing 50 mM ammonium acetate in the ratio 60:40 (v/v), and pH adjusted to 4.8 with orthophosphoric acid. The instrumental settings are a flow rate of 1.0 ml/min and detector wavelength at 263 nm. The retention times for nateglinide and metformin are 3.55 and 2.31 min, respectively. The method is validated and shown to be linear. The linearity range for nateglinide and metformin are 20-560 µg/ml respectively. The percentage recovery for nateglinide and metformin are 98.80-100.48 and 99.71-100.56 % respectively. The correlation coefficients of nateglinide and metformin are 0.999 and 0.999, respectively. The relative standard deviation for six replicates is always less than 2%....
Three simple and sensitive methods were developed for the determination of a mixture of amlodipine besilate (AM) and valsartan (VL) without prior separation. In methods (A), (B) and (C), AM was determined by the application of direct spectrophotometry technique and measuring its zero-order absorption spectra at 360 nm. While in method (A), VL was determined by the application of first derivative of ratio spectra technique (1DD) and measuring its amplitude at 255.5 and 290 nm. Method (B) was based on isosbestic point technique, where the total content of the mixture was determined at their isosbestic point at 242 nm, while the content of AM was determined as mentioned at 360 nm. Thus the content of VL could be calculated by subtraction. Method (C) was depended on the use of a new and precise ratio subtraction technique for the determination of VL at its λmax 250 nm in presence of AM, while the latter was determined as mentioned at 360 nm. Linearity range was 4 – 64 µg/ml for both AM and VL for the three methods. Since all methods were the same for AM. The proposed methods were proved using laboratory prepared mixtures of the two drugs and were successively applied for their analysis in tablet form....
Simultaneous spectrophotometric determination of Irbesartan (IRB) and Hydrochlorothiazide (HCZ) by H-Point standard addition method (HPSAM) and two chemometric methods Partial least square (PLS-1) and Principle Component regression (PCR) are described. The results of HPSAM showed that simultaneous determination could be performed with the ratio of 1:4 – 6:0.8 for Irbesartan – Hydrochlorothiazide. The chemometric approaches were successfully applied to quantify the two drugs in the mixture using the information included in the UV absorption spectra of appropriate solutions in the range of 200 – 350nm with the intervals = 1 nm at 151 wavelengths. The calibration or regression was obtained by using the absorbance data matrix and concentration data matrix for the prediction of the unknown concentrations of IRB and HCZ in their mixture. The linear range was found to be 1-5 µg/ml and 0.5-2.5 µg/ml in their mixture. The procedure did not require any separation step. The accuracy and precision of the methods were assessed. These methods were successfully applied to a pharmaceutical preparation, tablet and the results were compared with each other....
A highly selective, simple, sensitive and accurate high performance liquid chromatography method has been developed and validated for the simultaneous estimation of prazosin and H2 receptor antagonists (cimetidine, famotidine & ranitidine) in the bulk material, pharmaceutical formulation and human serum. The declaration of peaks were achieved on a Nuclosil®, 100-10, C-18 column (250×4.6mm, 10 micron) using methanol:water:acetonitrile (60:45:5 v/v, pH 3.83) as the mobile phase at a flow rate of 1mL min-1 effluents were monitored at 240 nm with a UV detector. In isocratic mode, the elution times of H2 receptor antagonists and prazosin were 2.88 ± 0.01 and 4.12 ± 0.02 minutes respectively. The, assay can be used as a routine analysis as the total eluting time for the two components is less than ten minutes. Validation of the proposed method was carried out as per International Conference on Harmonization (ICH) guidelines. The assay was linear from 2.5 to 50 μg mL-1 for prazosin and from 20 to 200 μg mL-1 for H2 receptor antagonists. The method was selective, precise, and accurate and can be used for routine analysis of pharmaceutical preparations, quality control and clinical laboratories....
A simple, economic, accurate reverse phase isocratic RPHPLC method was developed for the Simultanious estimation of Gliclazide 80mg & Rosiglitazone 2mg in Tablet dosage form. The quantification was carried out using Symmetry C18 (4.6 x 100mm, 5µm, Make:XTerra) with UV detected at 229 nm. The elution was achieved isocratically with a mobile phase comprises of mixture of buffer 500 mL (50%) and 500 mL of Acetonitrile HPLC (50%). The flow rate was 0.8ml/min The procedure was validated as per ICH rules for Accuracy, Precision, Detection limit, Linearity, Reproducibility and Quantitation limit. The linearity concentration range was 20-100ppm for Gliclazide and 10-50ppm for Rosiglitazone with the correlation coefficient of 0.999. The percentage recovery for Gliclazide & Rosiglitazone was found to be 100.6% and 101.2% respectively. Limit of detection values were found to be 0.002mcg/ml and 0.001mcg/ml respectively for Gliclazide & Rosiglitazone. Limit of quantitation values were found to be 0.009mcg/ml and 0.006mcg/ml respectively for Gliclazide & Rosiglitazone. The method has been successfully used to analyze commercial solid dosage containing Gliclazide & Rosiglitazone with good recoveries and proved to be robust....
A simple stability indicating reversed-phase HPLC method was developed and subsequently validated for simultaneous estimation of diacerein (DCN) and aceclofenac (ACF) present in pharmaceutical tablet dosage forms. The proposed RP-HPLC method utilizes a Lichrospher 100 C-18 RP column (250 mm × 4mm × 5 µm) in a isocratic separation mode with mobile phase consisting of acetonitrile and phosphate buffer in the proportion of 50:50 % (v/v), pH adjusted to 6.5 using 0.1 % v/v ortho phosphoric acid delivered at a flow rate 0.8 ml/min and the effluent was monitored at 254 nm. The retention time of DCN and ACF was found to be 2.50 and 3.35 min respectively. DCN, ACF and their formulation were exposed to acidic, alkaline, photolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. The described method was linear over a range of 0.05-50µg/ml for DCN and 0.2-100 µg/ml for ACF. The mean percentage recoveries were 101.28 and 99.81 for DCN and ACF respectively. 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 critical value....
Traditional medicines are effective but the Standardization of herbal formulations is essential in order to assess the quality of drugs, based on the concentration of their active principles. Department of AYUSH (Government of India) has given preliminary guidelines for standardizing these conventional formulations, for uniformity of batches in production of herbal formulation and it is necessary to develop methods for evaluation. The present work is an attempt to standardize Mehari choornam, a traditional ayurvedic formulation, used in reducing the blood sugar levels in border-line diabetes and also acts as on anti-oxidant thereby preventing end-organ complications. The various parameters performed included organoleptic characteristics, physicochemical, Microscopical and HPTLC analysis. The results obtained may be considered as tools for assistance to the regulatory authorities, scientific organizations and manufacturers for developing standards....
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