Current Issue : July - September Volume : 2012 Issue Number : 3 Articles : 13 Articles
UV- Spectrophotometric methods have been developed for estimation of Risagiline mesylate in bulk drug and in pharmaceutical formulation as it is not official in any pharmacopoeia. The linearity was found to be in the concentration range of 2-20μg/ml at 210nm, and 20-200μg/ml at 265nm and 272nm. Amounts of drug estimated from tablet formulation were in good agreement with label claim. The method was validated statistically and by recovery studies. The proposed methods are economical and sensitive for the estimation of Risagiline Mesylate (RM) in bulk and tablet dosage....
These days Slimming Herbal Medicinal Products (HMPs) are more in demand in Indian market and it encourages manufacture of Slimming HMPs to be adulterate the HMPs with active Synthetics to increase the efficiency of the products. Sibutramine is anorexic drug by acting on serotonin neurotransmitter. But Sibutramine is the drug which is recently banned due to few life threatening cardiac side effects. Sibutramine is one of the possible adulterant of the Slimming HMPs that can be added by the manufacturer and has to be detected by the analyst to determine the adulteration in the HMPs. The purpose of this study was to identify and quantify the Sibutramine in the Slimming HMPs in less time with accurate result. The new validated method was developed by HPTLC at 223 nm. HPTLC separation was performed on (10 X10 cm, 20 X 10 cm) Pracoated Silica Gel G60 F254 Aluminum sheets by using mobile phase Chloroform: Acetone: Methanol (8.5:1.0:0.55 v/v/v). In analysis linearity in the range of 300-2500 ng/band-1 and method was validated for accuracy, precision, Linearity, Specificity, Robustness and were successfully applied to the local marketed products. As a conclusion this method was found to be useful for the routine analysis of illegally added Sibutramine in the HMPs....
A simple, novel, sensitive, and specific spectrophotometric method was developed and validated for the determination of Metoprolol succinate and Clopidogrel bisulphate in tablet dosage form. First order derivative spectroscopy method is adopted to eliminate spectral interference. The method obeys Beer�s Law in concentration ranges selected for evaluation. Metoprolol succinate and Clopidogrel bisulphate have ?max at 223nm and 222.22 nm respectively in 0.1N HCL solvent. The method was validated for linearity, accuracy and precision as per ICH guidelines. The zero crossing point for Metoprolol succinte and Clopidogrel bisulphate was 245.76nm and 276.13nm respectively. The LOD and LOQ value were found to be 0.15 and 0.18 ?g/ml for Metoprolol succinate and 2 and 4.5 ?g/ml for Clopidogrel bisulphate respectively. The developed and validated method was successfully used for the quantitative analysis of combined tablet dosage form....
A Reversed-Phase High Performance liquid chromatographic (RP-HPLC) method was developed for the simultaneous determination of Ambroxol Hydrochloride and Olopatadine Hydrochloride in combined tablet dosage form. The analysis was carried out using Phenomenex Luna C18, pre-packed column. Mobile phase, containing Acetonitrile: 0.05 M Potassium Dihydrogen Ortho Phosphate Buffer (70: 30) pH adjusted to 7.1 with Tri ethyl Amine was pumped at a flow rate of 1.0 ml/min with UV-detection at 248 nm. Retention time was 4.95 ± 0.007 min and 2.84 ± 0.010 min for Ambroxol Hydrochloride and Olopatadine Hydrochloride, respectively. The method was validated for linearity, accuracy, precision, and specificity. The method showed good linearity in the range of 10 – 60 μg/ml for Ambroxol Hydrochloride and 10 – 60 μg/ml for Olopatadine Hydrochloride. The detection limit of the proposed method was found to be 2.16 μg/ml and 3.26 μg/ml and the quantification limit was 6.56 μg/ml and 9.87 μg/ml for Ambroxol Hydrochloride and Olopatadine Hydrochloride, respectively. The % recovery was within the range between 98.90 - 99.93 % and 99.93 - 101.24 % for Ambroxol Hydrochloride and Olopatadine Hydrochloride, respectively. The % RSD for precision and accuracy of the method was found to be less than 2%. The method was validated as per the ICH guidelines. The method was successfully applied for routine analysis of Ambroxol Hydrochloride and Olopatadine Hydrochloride in combined tablet dosage form....
An LC method involving a C18 column as stationary phase and a mixture of aqueous sodium dihydrogen phosphate (0.2 M; pH of the buffer adjusted to 6.3 ±0.1 with 3.6 % w/v sodium hydroxide solution) and methanol in the ratio (60:40, v/v) as mobile phase was developed for the effective separation of all degradation products. It involved 1ml min−1 flow rate and detection wavelength of 317 nm. The developed method was found to be precise, accurate, specific and selective. The drug showed instability in solution state under alkaline, photolytic and UV stress conditions, but was relatively stable in the acid, oxidative, neutral, dry and wet heat degradation. Primarily, maximum degradation products were formed under alkaline conditions. The products formed under different stress conditions were investigated by LC and the major degraded product of alkali degradation sample by LC & MS. In the MS of pure drug m/z values and fragmentation patterns matched with starting material used in synthesis. The alkaline degraded products were characterized through MS fragmentation studies. Based on the results, a more complete degradation pathway for the drug could be proposed....
Method for assay of Terbinafine HCl Present in topical Cream Formulation was developed and validated by RP-HPLC method. Testing was done by different Analytical columns such as C8, CN and C18 column. Finally good separation was achieved using Phenomenex C18 (250mm x 4.6mm, 5µ) used for analysis. The analysis time was 30 min and flow rate was 1 ml/min. Mobile phase used for chromatography was filtered and degassed mixture of Acetonitrile: Methanol: Water (40:10:50), 0.1 ml O-Phosphoric Acid and 0.1 ml of Triethalamine. UV detection was accomplished at 282 nm. The method was validated according to ICH guideline recommendation. The report demonstrates that this method is effective, simple, sensitive and Accurate for Assay of Terbinafine HCl in cream formulation....
A simple and sensitive HPTLC method has been developed for determination of Amlodipine besylate and Clopidogrel bisulphate in its pharmaceutical dosage forms. The method employed HPTLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. Hexane: Acetone: TEA (6.5:3:0.5 v/v) as a mobile phase. After that saturation time is optimized for the better separation The Rf value of Amlodipine besylate is 0.23±0.02 and of Clopidogrel bisulphate is 0.69±0.02 were found. The linearity for both the drugs were in the range of 50-350ng/band and 750-5250 ng/band. The % recoveries of Amlodipine besulate and Clopidogrel bisulphate were found to be in the range of 100.24-100.37 and 99.36-100.82 respectively. The proposed method was validated and successfully applied to the estimation of Amlodipine besylate and Clopidogrel bisulphate in combined dosage form....
Cefixime Trihydrate (CEF) a broad spectrum oral cephalosporin that was approved by USFDA in 1997 for the treatment of mild to moderate bacterial infections is marketed in combination with Dicloxacillin Sodium (DICLOXA), a narrow spectrum beta-lactam antibiotic of the penicillin class. CEF and DICLOXA were estimated at 254nm by densitometry using silica gel 60/UV254 as stationary phase and a premix of toluene: methanol: triethylamine (5:4:1 v/v) as mobile phase. The method was found linear in a range of 200-600 ng/band for CEF and 500-1500 ng/band for DICLOXA with a correlation coefficient 0.998 for both. CEF and DICLOXA were well resolved with Rf 0.26±0.02 and 0.57±0.02, respectively. The developed high performance thin layer chromatography method was found to be specific, precise and reproducible and can be used for the routine estimation of CEF and DICLOXA in the combined dosage form, available in market....
Simple, rapid, sensitive and accurate and reproducible reverse phase high performance liquid chromatographic (RP-HPLC) method was developed for estimation of Tapentadol Hydrochloride. Chromatography was carried out at ambient temperature and separation of this drug was achieved on C18 column (250*4.6mm*5µm) as stationary phase with a mobile phase comprising of methanol: water (70:30, pH-5), at flow rate 1.5 mL/min. The detection wavelength for tapentadol hydrochloride was 272 nm. The retention time of tapentadol hydrochloride 2.38 minute. The Linearity of tapentadol hydrochloride was in the range of 20-100 μg/ml (r2=0.997). The results of analysis have been validated statistically for linearity, LOD, LOQ, accuracy, precision and recovery studies of the proposed method. Present methods are economical and sensitive for the estimation of Tapentadol Hydrochloride in bulk and tablet dosage forms in routine manner....
A simple reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the simultaneous determination of Zonisamide and Lamotrigine in combined dosage form and human plasma. The separation was achieved using a Phenomenex 250 mm × 4.6 mm i.d., 5 μm particle size C18 column. Mobile phase containing a mixture of Methanol and phosphate buffer (pH 6.5) (60: 40 v/v) was pumped at a flow rate of 1.0 mL/min. UV detection was performed at 295 nm. The method was validated for accuracy, precision, specificity, linearity and sensitivity. The developed and validated method was successfully used for quantitative analysis of combined dosage form. The chromatographic analysis time was approximately 10 min per sample with complete resolution of Zonisamide (tR = 4.64 min.) and Lamotrigine (tR = 6.88 min). Validation studies were performed according to ICH Guidelines revealed that the proposed method is specific, rapid, reliable and reproducible. The calibration plots were linear over the concentration ranges 0.1 - 2.0 μg/mL and 0.6 - 2.4 μg/mL with LOD of 0.01 μg/mL and 0.05 μg/ml for both compounds and limits of quantification 0.1 μg/mL and 0.2 μg/mL for Zonisamide and Lamotrigine respectively. The developed method was successfully applied for the simultaneous analysis of the studied drugs in their combined form and human plasma. The mean percentage recoveries in were 99.547 ± 1.687 and 99.563 ± 1.674 for Zonisamide and Lamotrigine respectively. The method was found to be robust proved that there was no significant difference in the accuracy and precision....
A specific, sensitive, precise and stability-indicating high-performance liquid chromatographic method of analysis of albendazole both as a bulk drug and in formulation was developed and validated. The separation was achieved by using a mobile phase of methanol: water pH 3 (85:15, v/v) and Chromatopak Peerless Basic-RP-C18 column at flow rate of 1.0 ml/min. The detection was done at 230 nm. The retention time of albendazole was 6 ± 0.01 min. This method has been successively applied to pharmaceutical dosage form. No chromatographic interference from the tablet excipients was found. Albendazole was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The drug was found to be stable only under thermal stress conditions; also the degraded products were well resolved from the pure drug with significantly different retention time values. Linearity was found to be in the range of 5–30 µg/ml with significantly high value of correlation coefficient. The method was validated for precision, robustness and recovery. The limit of detection and quantitation were 0.59 µg/ml and 1.8 µg/ml. The acid and base degraded products of albendazole were subjected to GC-MS analysis. From the mass spectral data of degraded products, possible degradation pathways were outlined....
The present study deals with standardization of marketed herbal formulation Mustakarishta based on various parameters, TLC and HPTLC fingerprinting profiles. Mustakarishta was also prepared by in-house fermentation method as per procedure given in authorized books of Ayurveda following GMP guidelines. Raw herbal material was authenticated, standardized and used for preparation of arishta. It was found that results for all parameters that are tested were within acceptance criteria. Marker compound that isolated from raw plant mustaka and marketed Mustakarishta was characterized using spectral techniques. Both products were studied using fingerprint techniques by TLC and HPTLC in toulene: ethyl acetate (9:1 v/v) as mobile phase. Both techniques were found to be simple, rapid, reliable and economic....
The present article describes the development and validation of a Gas Chromatographic method for the confirmation of octacosanol in the mixture of policosanol. Literature cites the percentage of octacosanol in policosanol mixture to be up to 85% and no isomers have been reported as date. A gas chromatographic method using a packed column was developed and validated for determination of fatty alcohols in policosanol predominantly octacosanol. Typical concentration considered for this study was 0.1mg/ml or 100 PPM based on the range assay between 0.02mg/ml (20ppm) and 0.12mg/ml (120ppm). The validation steps included the verification of linearity, repeatability, specificity, recovery, reproducibility, stability and ruggedness in the samples. The method can detect degradation products and has good linearity (correlation coefficient 0.99) in a range of 20ppm to 150ppm (20% - 120%) and accuracy (recovery = 100.07 -101%). The nominal concentration considered for this method is 0.1mg/ml (100 ppm). The recoveries demonstrated in this method are 100.6% lowest at 120% and 50% of standard concentration and 101.6% at level of 100% of the standard (nominal) concentration with RSD not more than 2%. System precision and intermediate precision RSD was found to be not more than 2% while in intermediate precision the ratio between two determinations was found to be in between 0.97 and 1.03 Robustness was examined by changing operational parameters with RSD not more than 1%. Repeatability and reproducibility were obtained at a uniform level. These findings suggest good reproducibility and can be suitable for analyzing compositions containing policosanol for quality control and stability studies. The results of the validation process revealed that the proposed method is suitable for reliable quantification and confirmation of octacosanol content in the policosanol mixture and for analysis of tablets therein. The method is intended to be used for determination and identification/confirmation of octacosanol in policosanol (Assay determination) and capable of detecting degradation products, but may not be capable to resolve the individual impurities or degradation products....
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