scholarly journals Simple Spectrophotometric Determination of Torsemide in Bulk Drug and in Formulations

2008 ◽  
Vol 5 (3) ◽  
pp. 473-478 ◽  
Author(s):  
Marothu Vamsi Krishna ◽  
Dannana Gowri Sankar

A simple and cost effective spectrophotometric method is described for the determination of torsemide in pure form and in pharmaceutical formulations. The method is based on the formation of blue colored chromogen when the drug reacts with Folin-Ciocalteu (F-C) reagent in alkaline medium. The colored species has an absorption maximum at 760 nm and obeys beer's law in the concentration range 30 – 150 ug mL−1. The absorbance was found to increase linearly with increasing concentration of TSM, which is corroborated by the calculated correlation coefficient value of 0.9999 (n=8). The apparent molar absorptivity and sandell sensitivity were 1.896×103L mol−1cm−1and 0.183 μg cm−2, respectively. The slope and intercept of the equation of the regression line are 5.4x10−3and 1.00×10−4respectively. The limit of detection was 0.94.The optimum experimental parameters for the reaction have been studied. The validity of the described procedure was assessed. Statistical analysis of the results has been carried out revealing high accuracy and good precision. The proposed method was successfully applied to the determination of TSM in pharmaceutical formulations.

2010 ◽  
Vol 7 (2) ◽  
pp. 551-554 ◽  
Author(s):  
R. Vijayalakshmi ◽  
P. Bhargavi ◽  
P. Srujana Kumari ◽  
P. Sruthi ◽  
M. D. Dhanaraju

A simple and cost effective spectrophotometric method is described for the determination of ceftibuten in pure form and in pharmaceutical formulations. The method is based on the formation of blue colored chromogen, when the drug reacts with Folin-Ciocalteu (F-C) reagent in alkaline medium. The colored species has an absorption maximum at 798 nm and obeys Beer’s law in the concentration range 10-50 mcg/mL. The apparent molar absorptivity and sandell’s sensitivity were 0.4583x104and 0.3x104respectively. The slope and intercept of the equation of the regression line are 4.5x10-3and 1.3x10-5respectively. The optimum experimental parameters for the reaction have been studied and the validity of the described procedure was assessed. Statistical analysis of the results has been carried out revealing high accuracy and good precision. The proposed method was successfully applied for the determination of ceftibuten in pharmaceutical formulations.


2009 ◽  
Vol 6 (4) ◽  
pp. 1233-1239 ◽  
Author(s):  
J. Saminathan ◽  
A. S. Sankar ◽  
K. Anandakumar ◽  
T. Vetrichelvan

A simple and cost effective spectrophotometric method is described for the determination of fluvastatin sodium in pure form and in pharmaceutical formulations. When the drug reacts with sodium hydroxide shows absorption maximum at 304 nm and obeys beer's law in the concentration range 5-25 µg mL-1. The absorbance was found to increase linearly with increasing concentration of FVS, which is corroborated by the calculated correlation coefficient value of 0.9999 (n=5). The apparent molar absorptivity and sandell sensitivity were 1.1905×104and 0.0368844 µg cm-2cm respectively. The slope and intercept of the equation of the regression line are 0.027112 and 0.003539 respectively. The limit of detection and limit of quantification was found to be 0.0811 µg mL-1& 0.2460 µg mL-1. The validity of the described procedure was assessed. Statistical analysis of the result has been carried out revealing high accuracy and good precision. The proposed method was successfully applied to the determination of FVS in pharmaceutical formulations without any interference from common excipients. The relative standard deviations were ≤ 0.937%, with recoveries of 98.60% -101.70%.


2007 ◽  
Vol 4 (2) ◽  
pp. 173-179 ◽  
Author(s):  
K. Basavaiah ◽  
U. R. Anil Kumar

A simple spectrophotometric method is proposed for the determination of zidovudine(ZDV) in bulk drug and in pharmaceutical preparations. The method is based on the oxidation of ZDV by a known excess of oxidant N-bromosuccinimide (NBS), in buffer medium of pH 1.5, followed by the estimation of unreacted amount of oxidant with metol and sulphanilic acid. The reacted oxidant corresponds to the amount ZDV. The purple-red reaction product absorbs maximally at 530 nm and Beer’s law is obeyed over a range 5 to 75 μg mL-1. The apparent molar absorptivity is calculated to be 5.1×103L mol-1cm-1, and the corresponding Sandell sensitivity value is 0.052 μg cm-2. The limit of detection and quantification are found to be 0.90 and 2.72, respectively. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The method was successfully applied to the assay of ZDV in tablet/capsule preparations and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common tablet/capsule excipients. The accuracy of the method was further ascertained by performing recovery studies via standard-addition method.


2018 ◽  
Vol 33 (2) ◽  
pp. 21
Author(s):  
Kanakapura Basavaiah ◽  
Okram Zenita Devi

Two sensitive spectrophotometric methods are described for the determination of simvastatin (SMT) in bulk drug and in tablets. The methods are based on the oxidation of SMT by a measured excess of cerium (IV) in acid medium followed by determination of unreacted oxidant by two different reaction schemes. In one procedure (method A), the residual cerium (IV) is reacted with a fixed concentration of ferroin and the increase in absorbance is measured at 510 nm. The second approach (method B) involves thereduction of the unreacted cerium (IV) with a fixed quantity of iron (II), and the resulting iron (III) is complexed with thiocyanate and the absorbance measured at 470 nm. In both methods, the amount of cerium (IV) reacted corresponds to SMT concentration. The experimental conditions for both methods were optimized. In method A, the absorbance is found to increase linearly with SMT concentration (r = 0.9995) whereas in method B, the same decreased (r = -0.9943). The systems obey Beer’s law for 0.6-7.5 and 0.5-5.0 μg mL-1 for method A and method B, respectively. The calculated molar absorptivity values are 2.7 X 104 and 1.06 X 105 Lmol-1 cm-1, respectively; and the corresponding sandel sensitivity values are 0.0153 and 0.0039μg cm-2, respectively. The limit of detection (LOD) and quantification (LOQ) are reported for both methods. Intra-day and inter-day precision, and accuracy of the methods were established as per the current ICH guidelines. The methods were successfully applied to the determination of SMT in tablets and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common excipients added to tablets. The accuracy and validity of the methods were further ascertained by performing recovery experiments via standard addition procedure.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Kumble Divya ◽  
Badiadka Narayana ◽  
Majal Sapnakumari

A new spectrophotometric method is developed for the determination of Paracetamol (PCT) and protriptyline HCl (PTP) in pure forms and in pharmaceutical formulations. The experiment involves the use of 3-chloro-7-hydroxy-4-methyl-2H-chromen-2-one as a novel chromogenic reagent for the determination of PCT and PTP. The method is based on the formation of charge transfer complex between the drugs and chromogenic reagent. Beer's law is obeyed in the concentration ranges 10.00–60.00 µg mL−1 for PCT at 545 nm and 40.00–160.00 µg mL−1 for PTP at 468 nm. The molar absorptivity, Sandell, sensitivity, and limit of detection and quantification are also calculated. The method has been successfully applied for the determination of both PCT and PTP in pharmaceutical samples with acceptable results.


2007 ◽  
Vol 4 (2) ◽  
pp. 272-278 ◽  
Author(s):  
Marothu Vamsi Krishna ◽  
Dannana Gowri Sankar

Three simple, sensitive and cost effective Spectrophotometric methods are described for the determination of pitavastatin calcium (PST) in bulk drugs and in pharmaceutical formulations. These methods are based on the oxidation of PST by ferric chloride in presence ofo-phenanthroline (Method A) or 2, 2’ bipyridyl (Method B) or potassium ferricyanide (Method C). The colored complex formed was measured at 510, 530 and 755 nm for method A, B and C respectively against the reagent blank prepared in the same manner. The optimum experimental parameters for the color production are selected. Beer’s law is valid with in a concentration range of 4-20 μg mL-1for method A, 7.5-37.5 μg mL-1for method B and 5 -25 μg mL-1for method C. For more accurate results, ringbom optimum concentration ranges are 5-18 μg mL-1for method A , 8.5-35.5 μg mL-1for method B and 6.0-23.0 μg mL-1for method C. The molar absorptivities are 3.55x104, 2.10x104and 3.10x104L mol-1cm-1. Where as sandell sensitivities are 0.024, 0.041 and 0.028 μg cm-22 for method A, B and C respectively. The mean percentage recoveries are 99.95 for method A, 101.35 for method B and 100.33 for method C. The developed methods were applied for the determination of PST in bulk powder and in the pharmaceutical formulations without any interference from tablet excipients.


2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagib A. S. Qarah ◽  
Sameer A. M. Abdulrahman

Two simple methods are described for the determination of ethionamide (ETM) in bulk drug and tablets using cerium (IV) sulphate as the oxidimetric agent. In both methods, the sample solution is treated with a measured excess of cerium (IV) solution in H2SO4 medium, and after a fixed standing time, the residual oxidant is determined either by back titration with standard iron (II) solution to a ferroin end point in titrimetry or by reacting with o-dianisidine followed by measurement of the absorbance of the orange-red coloured product at 470 nm in spectrophotometry. In titrimetry, the reaction proceeded with a stoichiometry of 1 : 2 (ETM : Ce (IV)) and the amount of cerium (IV) consumed by ETM was related to the latter’s amount, and the method was applicable over 1.0–8.0 mg of drug. In spectrophotometry, Beer’s law was obeyed over the concentration range of 0.5–5.0 μg/mL ETM with a molar absorptivity value of 2.66 × 104 L/(mol·cm). The limits of detection (LOD) and quantification (LOQ) calculated according to ICH guidelines were 0.013 and 0.043 μg/mL, respectively. The proposed titrimetric and spectrophotometric methods were found to yield reliable results when applied to bulk drug and tablets analysis, and hence they can be applied in quality control laboratories.


2018 ◽  
pp. 49-55
Author(s):  
Y. M. Zhuk ◽  
S. O. Vasyuk

In this investigation a visible spectrophotometric method for the determination of sotalol based on the absorbance of colored product of the reaction between sotalol hydrochloride and bromcresol purple in acetone medium at 399 nm measurement was developed. The optimal conditions for the quantitative determination of sotalol hydrochloride in the content of pharmaceutical drugs were established. The stoichiometric relationship coefficients between sotalol hydrochloride and bromcresol purple were determined. The validation of the worked out procedure on such validated characteristics as linearity, precision, accuracy and robustness was carried out. The aim. To develop a highly sensitive, easy to use, cost-effective and valid method for quantitative determination of sotalol hydrochloride in dosage forms. The analysis method. Visible spectrophotometry. The analytical parameters such as molar absorptivity, Beer’s law limits and Sandell’s sensitivity values were calculated. The developed methods give the result with repeatability sufficient for dependable determination the investigated substance in pharmaceutical formulations. Accuracy established by analyte addition technique. Determined factors that influence on the absorbance value: reagent quantity and timing stability. Sample solutions stable during 30 min. Addition to sample solution ± 10% bromcresol purple solution is not change the absorbance value. Established that reaction between sotalol hydrochloride and bromcresol purple proceeds in acetone medium at room temperature. Molar absorption coefficient is 2,62∙103.


Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3115 ◽  
Author(s):  
Alina Pyka-Pająk ◽  
Małgorzata Dołowy ◽  
Wioletta Parys ◽  
Katarzyna Bober ◽  
Grażyna Janikowska

A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validated as per ICH guidelines by specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. Method validations indicate a good sensitivity with a low value of LOD and LOQ of both examined active substances. The linearity range was found to be 1.50–9.00 μg/spot and 1.50–13.50 μg/spot for acetylsalicylic and ascorbic acid, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of combined tablet formulation equal 97.1% and 101.6% in relation to the label claim that acetylsalicylic acid and ascorbic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine simultaneous analysis of acetylsalicylic acid and ascorbic acid in combined pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography in the quality control of above-mentioned substances, and it can be applied when HPLC or GC is not affordable in the laboratory.


2011 ◽  
Vol 8 (1) ◽  
pp. 281-287 ◽  
Author(s):  
K. Srikanth ◽  
K. A. Emmanuel

In the present study, two simple, sensitive and reproducible visible spectrophotometric methods were developed for the determination of reboxetine in pure form and in pharmaceutical formulations. The methods involve acid hydrolysis of reboxetine methane sulphonate (Reboxetine as methane sulphonate) and the product obtained was used for the estimation. Out of the two methods developed in the laboratory, the first method involves the condensation reaction of hydrolysed reboxetine methane sulphonate with ethyl acetoacetate in sulphuric acid medium and the second method involves the diazocoupling reaction of hydrolysed reboxetine methane sulphonate with diazotizedp-sulphanilic acid in alkaline medium. They have absorption maxima at 400 nm and 430 nm respectively and obey Beer’s law in the concentration ranges of 0.5 - 0.3 μgmL-1and 1.0 - 7.5 μgmL-1respectively. Results of analysis were validated statistically and by recovery studies. The apparent molar absorptivity values (∈max) obtained are 7.549 x 104L mol-1cm-11 and 2.656x104Lmol-1cm-1respectively. Both these have correlation coefficient value of 0.9999. The proposed methods have good precision and accuracy.


Sign in / Sign up

Export Citation Format

Share Document