Current Issue : April - June Volume : 2014 Issue Number : 2 Articles : 12 Articles
A simple, reproducible and cost effective spectroscopic method developed and validated for ambrisentan in bulk and tablet dosage form. The drug was determined by using Acetonitrile as diluent at 260nm. Validation was performed as ICH guidelines for linearity, accuracy, precision, LOD and LOQ. The %recovery study for the proposed method was ranged between 99.21% and 99.67% indicating no interferences of the tablet excipients. Linearity was obtained in concentration range of 10-80�µg/ml for ambrisentan with correlation coefficient of 0.9996 and regression equation was found to be y=0.0124x.0019. The LOD and LOQ were found to be 0.48�µg/ml and 1.46�µg/ml respectively by simple UV spectroscopy....
New three high performance liquid chromatography (HPLC) -chemometric combinations were implemented for the simultaneous determination of ibuprofen and famotidine in tablets. Three chemometric calibration techniques; classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS) were applied to the ratio of peak areas at multiwavelength using Diode Array Detector (DAD) responses at 245nm, 250nm, 255nm, 260nm and 265 nm. These combinations were called HPLC-CLS, HPLC-PCR and HPLC-PLS. For comparison purposes, a new validated developed classic HPLC method was used to confirm the results obtained from HPLC-chemometric calibration techniques. A good chromatographic separation between the two drugs with ketoprofen as an internal standard (IS) was achieved using a C18 column 5 Ã?µm, 4.6Ã?â??250 mm and a mobile phase containing 20 mM acetate buffer (pH=3) and methanol [v/v, 25: 75] at flow rate 1.8 ml/ min. Run time was found to be less than 5 minutes. The classic HPLC method was carried out at 255 nm. The developed methods were applied to the quantitative analysis of the investigated drugs in their synthetic mixtures and in tablets. The developed HPLC-chemometric techniques overcome the main problems of the classic HPLC method such as separation treatment, the optimization of experimental conditions and selection of one specific wavelength. HPLC-chemometric techniques using DAD do not require tedious validation steps and eliminate the errors of single regression equations based on single wavelength and provide reliable results with high sensitivity, accuracy and robustness as well as high purity assessment via DAD empowered by PCR and PLS....
Simultaneous spectrophotometric methods are described for the determination of losartan potassium, hydrochlorothiazide and amlodipine besylate in tablets using absorbance correction-H-Point Standard addition method (HPSAM) and partial least squares regression (PLS). A simple and novel method absorbance correction–HPSAM is reported for simultaneous estimation of three drugs using uv-visible spectrophotometry without any prior separation of samples. PLS regression can allow simultaneous spectrophotometric determination of several elements as well as improve the data handling process of complex chemical systems. The linear range was 1-5 µg/ml for losartan and hydrocholrothiazide and 2-10 µg/ml for amlodipine besylate. The relative standard deviation (RSD) for the simultaneous determination of 3 µg/ml of losartan, hydrochorothiazide and amlodipine by applying HPSAM was 1.249, 0.631 and 0.829 respectively. The total relative standard error for applying PLS method to 10 synthetic samples in the linear ranges of these drugs was ranging from 0.018 – 0.045 for all three drugs. The reported methods HPSAM and PLS can be claimed as green analytical chemistry as it does not involve the use of organic solvents and hence can be utilized for the routine analysis of these drugs from tablets....
A simple, accurate, precise and specific spectrophotometric method has been developed for the estimation of pirfenidone (PIR) in its tablet dosage form by using methanol as a solvent. The method is calibration graph method which involves estimation of PIR by taking absorbance at 317nm. This method follows Beer’s linearity in the range of 4-28 μg/ml. The mean % recovery was found to be in the range of 99.31–99.86 % for PIR. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of PIR in its tablet dosage form....
Glimepiride is antidiabetic drug and Ezetimibe is cholesterol absorption inhibitor.The combination of this two drug is used for the treatment of hypercholesterolemia.Two new, simple, accurate and precise uv spectrophotometric methods have been developed amd validated for the simultaneous determination of Glimepiride (GLM) and Ezetimibe (EZE) in their combine dosage forms. The first method is based on the simultaneous equations for analysis of both the drugs using methanol as solvent. Glimepiride has absorbance maxima at 228 nm and Ezetimibe has absorbance maxima at 247 nm in methanol. The second method is first order derivative method and wavelengths selected for quantitation were 234 nm for Glimepiride( zero crossing point for Ezetimibe) and 228 nm for Ezetimibe(zero crossing point for Glimepiride).The linearity was obtained in the concentration range of 6-16 μg/ml for both the drug. Both methods were validated statistically and recovery studies carry out.The method was successfully applied to tablet Dosage Form because no interference from the mixture excipients was found. The suitability of this method for the quantitative determination of Glimepiride and Ezetimibe was proved by validation. The proposed method was found to be simple and sensitive for the routine quality control application of Glimepiride and Ezetimibe in combination. The results of analysis have been validated statistically and by recovery studies.The validation study is statistically significant as all statistical parameter are within the acceptance range (% RSD < 2.0 and S.D. < 2.0) for both accuracy and precision....
Without resolving mixture of Ciprofloxacin and Phenylephrine Hydrochloride, simultaneous estimation has been successfully achieved by spectrophotometry. First method, simultaneous equations method employed formation and solving of mathematical simultaneous equations using 272 nm and 238 nm as the λmax of Ciprofloxacin and Phenylephrine Hydrochloride respectively in 0.1 M NaOH. Second method is first order derivative spectroscopy; wavelengths selected for quantitation were 262 nm for Ciprofloxacin (zero crossing point for Phenylephrine Hydrochloride) and 296 nm for Phenylephrine Hydrochloride (zero crossing point for Ciprofloxacin). These methods were validated as per ICH guidelines. Calibration curves were linear over the concentration ranges of 1-12 μg/ml and 5-30 μg/ml for Ciprofloxacin and Phenylephrine Hydrochloride respectively for both the methods. The validation study was statistically significant as all the statistical parameters were within the acceptance range (% RSD < 2.0 and S.D. < 2.0) for both accuracy and precision. The methods are successfully applied to pharmaceutical formulation, with no interference from excipients as indicated by the recovery study. The proposed methods are simple, rapid, economic and accurate for routine simultaneous estimation of Ciprofloxacin and Phenylephrine hydrochloride....
A simple, precise and accurate spectrophotometric method has been developed for simultaneous estimation of beclomethasone dipropionate and formoterol fumarate dihydrate using Q-absorption equation method. λmax of beclomethasone dipropionate and iso-absorptive point were found to be 239.2 nm and 232 nm respectively using methanol. Beer’s lambert’s law was obeyed over the concentration range of 1-6 μg/ml and 10-50 μg/ml for formoterol fumarate dihydrate and beclomethasone dipropionate respectively. A method is successfully applied on rotacaps. Developed methods were validated according to ICH guidelines....
Impatiens balsamina (syn. terada; garden balsam; garden jewelweed, sanskrit: “dushparijati”) belongs to the family balsaminaceae. This species has been used as indigenous traditional medicine in Asia for rheumatism, fractures and other ailments. In Korean folk medicine this impatiens species is used as a medicine called bong seon wha dae for the treatment of constipation and gastritis. It has been used for disease and skin afflictions. Juice from the leaves is used to treat warts and snakebite and the flower is applied to burns. Literature survey revealed that lawsone, a naphthoquinone, isolated from the methanolic extract of Impatiens balsamina leaves possesses potent antioxidant and anticancer activity [1] but it showed poor oral bioavailability. Hence, it was thought worthwhile to form a herbomineral complex of lawsone with zinc in order to improve the bioavailability and therapeutic activity of the phytoconstituents. The current research article deals with formation of herbomineral complex of lawsone and zinc, confirmation of formation of lawsone-zinc complex through physical properties and spectral analysis like UV- spectroscopy, IR, NMR, mass spectroscopy. It was prepared with an intention to increase bioavailability and bioactivity of lawsone....
Current research work describe rapid high performance thin layer chromatographic determination of Artesunate and Mefloquine form its combined pharmaceutical formulation. The mention drugs were spotted on silica gel F254 TLC plates under pure nitrogen stream by Linomat TLC spotter. Separation was carried out by using methanol, toluene, Ethyl acetate, and glacial acetic acid as mobile phase in ratio of 1:4.5:4:0.1 v/v/v/v. Developed TLC plates were scanned by CAMAG TLC scanner and detection was carried out at 235 nm. Rf value of separated drugs was found to be 0.235 and 0.537 for Artesunate and Mefloquine respectively. The developed method was validated as per ICH guidelines by studying various validation parameters like Accuracy, Precision, Robustness, LOD, LOQ and solvent stability. The developed and validated method was successfully applied for determination of Artesunate and Mefloquine from its combined pharmaceutical formulation....
Diethylcarbamazine citrate is an anthelmintic used in the treatment of filarial infections. Two rapid, simple, sensitive and selective spectrophotometric methods are presented for the determination of diethylcarbamazine citrate in pharmaceuticals. The methods are based on the formation of chloroform soluble 1:1 ion pair complexes (diethylcarbamazine citrate base: dye) formed between diethylcarbamazine citrate base and Sulfonphthalein dyes, bromophenol blue BPB, (method A) and bromothymol blue BTB, (method B). The complexes formed were measured directly (without extraction) at 430 nm (method A) and 440 nm (method B). The experimental conditions were optimized and the systems obey Beer’s law for 0.2-9.0 and 0.4–14.0 g ml-1 diethylcarbamazine citrate base for method A and method B respectively. The molar absorptivity and sandell sensitivity were calculated to be 4.985 × 104 l mol -1 cm-1 and 0.0079 ng cm-2, 3.152 × 103 l mol-1 cm-1 and 0.0124 ng cm-2 using BPB and BTB, respectively. The limits of detection and quantification were calculated to be 0.12 and 0.35; 0.08 and 0.24 g ml-1 using BPB and BTB respectively. The relative standard values for intra-day and inter-day precision were less than 3% and the accuracy was better than 3% for both methods. The methods were successfully applied to the determination of diethylcarbamazine citrate base in formulations with mean percentage assay values in the 98.6 to 102.5 range with standard deviation being less than 2%. The accuracy of the methods was further ascertained by parallel determination using the official method and by recovery studies....
Two simple, economic and highly sensitive uv-spectrophotometric methods have been described for the determination of rizatriptan benzoate (RTB) in bulk drug and in tablets. The proposed methods are based on the measurement of the absorbance of RTB either in 0.1 M HCl (method A) or in 0.1 M NaOH (method B) at 226 nm. Linearity was found to be in the ranges, 0.4-10.0 and 0.25-10.0 µg/ml RTB, for method A and method B, respectively with apparent molar absorptivity values of 5.01 x 104 and 6.09 x 104 l/mol/cm. The sandell sensitivity values, limits of detection (LOD) and quantification (LOQ) values have also been reported for both the methods. The proposed methods were successfully applied to the determination of RTB in tablets with good accuracy and precision and without detectable interference from common excipients. The validity and reliability of the proposed methods were further assessed by performing recovery studies via standard addition method. The degradation behaviour of RTB was investigated by subjecting it to different ICH prescribed stress studies like dry heat treatment, UV-degradation, acid hydrolysis, alkali hydrolysis and wet oxidation. The drug undergoes significant degradation under oxidation condition only. No degradation was observed under other stress conditions....
The present work describes zero absorbance spectrophotometric method for simultaneous estimation of ethamsylate and tranexamic acid in combined tablet dosage form. The developed method involve derivatization procedure for making tranexamic acid UV detectable. It employs development of zero absorbance method using two wavelengths 302.0 nm and 569 nm. The method obeys beer’s law in the employed concentration range of 20-70 μg ml-1 for both drugs. Results of analysis were validated statistically and by recovery studies....
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