New, simple and validated UV-spectrophotometric methods for the estimation of sodium usnate in preparations

2010 ◽  
Vol 29 (2) ◽  
pp. 157 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Ivan Savić ◽  
Saša Zlatković ◽  
Dragiša Djokić

New, simple, cost effective, accurate and reproducible UV-spectrophotometric methods were developed and validated for the estimation of sodium usnate in pharmaceutical preparations. Sodium usnate was estimated at 290 nm in water and phosphate buffer (pH 3):methanol (11:20 V/V). Beer’s law was obeyed in the concentration range of 0.1–5 μg·cm−3 (r = 0.997) in water and 1–12 μg·cm−3 (r = 0.999) in the phosphate buffer:methanol. The apparent molar absorptivity and Sandell’s sensitivity coefficient were found to be 3.16×104 dm3·mol−1·cm−1 and 11.58 ng·cm–2/0.001 A in water and 3.72×104 dm3·mol−1·cm−1 and 9.83 ng·cm–2/0.001 A in phosphate buffer:methanol, respectively, indicating the high sensitivity of the proposed methods. These methods were tested and validated for various parameters according to ICH guidelines. The detection and quantitation limits were found to be 0.0721 and 0.2163 μg·cm–3 in water and 0.163, 0.489 μg·cm−3 in phosphate buffer:methanol, respectively. The proposed methods were successfully applied for the determination of sodium usnate in pharmaceutical preparations. The results demonstrated that the procedure is accurate, precise and reproducible (R.S.D. < 2 %).

2014 ◽  
Vol 2014 ◽  
pp. 1-11 ◽  
Author(s):  
N. Swamy ◽  
K. N. Prashanth ◽  
K. Basavaiah

Two spectrophotometric methods are described for the determination of isoniazid (INH) in pharmaceuticals. In the first method (FCR method), INH is reacted with Folin-Ciocalteu reagent in Na2CO3 medium and the resulting blue colored chromogen measured at 760 nm. Iron(II), formed as a result of reaction between INH and iron(III), is made to react with ferricyanide, and the resulting Prussian blue is measured at 760 nm, basing the second method (FFC method). The conditions for better performance are optimized. Beer’s law is obeyed in the concentration ranges 0.5–10 and 0.2–3.0 μg mL−1 for FCR method and FFC methods, respectively, with corresponding molar absorptivity values of 1.12×104 and 4.55×104 L mol−1 cm−1. The methods are validated for accuracy, precision, LOD, LOQ, robustness, and ruggedness as per the current ICH guidelines. The validated methods were successfully applied to quantify INH in its commercial formulation with satisfactory results; hence the methods are suitable for isoniazid determination in bulk drugs and pharmaceuticals.


2008 ◽  
Vol 14 (3) ◽  
pp. 185-190
Author(s):  
Kanakapura Basavaiah ◽  
Urdigere Kumar ◽  
Kalsang Tharpa

Three new, simple, and cost-effective visible spectrophotometric methods are proposed for determination of gatifloxacin (GTF) using bromate-bromide mixture, and three dyes, methyl orange, indigocarmine and thymol blue, as reagents. The methods engross the addition of a known excess of bromate-bromide mixture to GTF in hydrochloric acid medium followed by determination of residual bromine by reacting with a fixed amount of either methyl orange and measuring the absorbance at 520 nm (method A) or indigo carmine and measuring the absorbance at 610 nm (method B) or thymol blue and measuring the absorbance at 550 nm (method C). In all the methods, the amount of bromine reacted corresponds to the amount of GTF, and the absorbance is found to increase linearly with the concentration of GTF. Under the optimum conditions, GTF could be assayed in the concentration range 0.25-1.5, 0.5-6.0, and 0.5-10 mg/mL by method A, method B and method C, respectively. The apparent molar absorptivities are calculated to be 1.6x105, 4.0x104 and 3.2x104 L mol-1 cm-1 for the method A, method B and method C, respectively, and the corresponding Sandell sensitivity values are 0.0025, 0.010 and 0.012 ?g/cm2. The intra-day and inter-day precision, and the accuracy of the methods were evaluated as per the current ICH guidelines. The methods were successfully applied to the determination of GTF in pharmaceutical preparations without the interference from any of the pharmaceutical adjuvant.


1997 ◽  
Vol 80 (6) ◽  
pp. 1368-1373 ◽  
Author(s):  
Kailasam Srtvidya ◽  
Natesan Balasubramanian

Abstract An easy and sensitive spectrophotometric assay of pyridoxine is described. The procedure is based on formation of an azo dye by the reaction of pyridoxine with diazotized 2,4-dinitroaniline followed by the reaction of the dye with Hg2+ ions to form a stable complex with maximum absorbance at 545 nm. The system obeys Beer’s law for 4–75 μg pyridoxine hydrochloride in an overall aqueous volume of 25 mL (correlation coefficient, 0.9998). On extraction into 5 mL butan-1-ol, the system obeys Beer’s law in the range 0.8–15 μg pyridoxine hydrochloride at 545 nm. The color is stable for 60 min in both aqueous and organic phases (molar absorptivity, 3.7 × 104 L/mol · cm; coefficient of variation, 3.1%, n = 10). The pyridoxine contents of pharmaceutical preparations, a processed foodstuff, and 2 rice samples were determined by using the proposed method. Assay reliability was established by recovery studies and parallel determination using a reported method.


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.


2012 ◽  
Vol 2012 ◽  
pp. 1-6
Author(s):  
Divya N. Shetty ◽  
B. Narayana

Two simple spectrophotometric methods are described for the determination of carvedilol (CAR). Method A is the condensation reaction of CAR with p-dimethylaminobenzaldehyde (PDAB), and the reaction mixture exhibits maximum absorbance at 601 nm. Method B is based on the charge transfer complex formation of CAR with p-chloranil; the color developed is measured at 662 nm. The calibration graphs are found to be linear over 50.00–250.00 and 20.00–100.0 μg mL−1 with molar absorptivity values of 0.92×103 and 0.257×104 L mol−1cm−1 for CAR-PDAB and CAR-p-chloranil, respectively. Statistical comparisons of the results are performed with regard to accuracy and precision using Student’s t-test and F-test at 95% confidence level. The methods are successfully employed for the determination of CAR in pharmaceutical preparations, and the results agree favorably with the reference and proposed methods.


2005 ◽  
Vol 2 (1) ◽  
pp. 6-14 ◽  
Author(s):  
K. Suvardhan ◽  
S. Ramanaiah ◽  
K. Suresh Kumar ◽  
D. Rekha ◽  
Umayur Bhagan ◽  
...  

Facile and sensitive spectrophotometric methods for the determination of trace and ultra trace amounts of chromium (VI) are described. 4-aminoantipyrine (APP) reacts with 1-naphthol (NPL) in presence of oxidising agent potassium dichromate in acidic medium to produce red coloured product having λmaxof 485 nm. The molar absorptivity and Sandell's sensitivity were 2.07x104l mol-1cm-1and 0.00240 μg/cm2respectively. The colour is stable for more than 6 h. The system obeys Beer's law in the range, 2-18 μg for determination of chromium (VI). The detection limits of chromium (VI) is 0.048 μg mL-1. The method is highly reproducible and has been applied to the analysis of chromium in synthetic, natural water samples and pharmaceutical preparations and the results compared favourably with the reported method.


Author(s):  
MALAK Y. AL BATHISH ◽  
AZZA A. GAZY ◽  
MARWA K. EL JAMAL

Objective: To develop and validate new, selective spectrophotometric colorimetric analytical methods for the quantification of methimazole in its pure form and in its pharmaceutical preparations. Methods: Method A is based on the oxidation of methimazole with potassium permanganate in alkaline medium, the manganate ion produced was measured at λmax= 610 nm. Method B is a kinetic determination of methimazole using fixed-time method based on the oxidation of methimazole using known excess of cerium (IV) nitrate in acidic medium and assessing the unreacted Ce (IV) by adding a fixed amount of methyl orange and measuring the absorbance of the resultant solution at λmax=507 nm which is equivalent to the unreacted methyl orange. The reaction conditions and analytical parameters are investigated and optimized. Method validation was carried out according to ICH guidelines in terms of linearity, LOD, LOQ, precision, and accuracy. Results: Beer’s law is obeyed in the range of 1.50–15.00 μg/ml for method A and 0.25–3.00 μg/ml for method B. The developed methods were subjected to the detailed validation procedure. The proposed spectrophotometric methods were applied for the determination of the methimazole in its pure form and in its pharmaceutical formulation. The percentage recoveries were found to be 100.82 % and 99.85 % in the pharmaceutical formulation for the two proposed methods, respectively. Conclusion: Both developed spectrophotometric methods, considered as green analytical chemistry, were found to be novel, highly selective and can be applied for the quality control of methimazole in its pure form and in its pharmaceutical formulation based on the simplicity, applicability of the parameters, accessibility of the reagents employed and reasonably low time of analysis.


2011 ◽  
Vol 76 (11) ◽  
pp. 1551-1560 ◽  
Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiah ◽  
Kanakapura Vinay

Two simple, rapid, cost-effective and sensitive spectrophotometric procedures are proposed for the determination of hydroxyzine dihydrochloride (HDH) in pharmaceuticals and in spiked human urine. The methods are based on the charge transfer complexation reaction of the drug with either iodine (I2) as a ?-acceptor (method A) in dichloromethane or picric acid (PA) as a ?-acceptor (method B) in chloroform. The coloured products exhibit absorption maxima at 380 and 400 nm for I2 and PA, respectively. The Beer Law was obeyed over the concentration ranges of 1.25-15 and 3.75-45 ?g mL-1 for method A and method B, respectively. The molar absorptivity values, Sandell sensitivities, limits of detection (LOD) and quantification (LOQ) are reported. The accuracy and precision of the methods were evaluated on intra-day and inter-day basis. The proposed methods were successfully applied for the determination of HDH in tablets and spiked human urine.


2006 ◽  
Vol 89 (4) ◽  
pp. 966-971 ◽  
Author(s):  
ArmaĞan Önal ◽  
Ş. Evrim Kepeki ◽  
S MÜge Çetin ◽  
Sidika ErtÜrk

Abstract Simple and reproducible spectrophotometric methods have been developed for determination of sertraline, fluoxetine, and venlafaxine in pharmaceutical preparations. The methods are based on the reactions between the studied drug substances and ion-pair agents (bromothymol blue, bromocresol green, or bromophenol blue) to produce yellow-colored ion-pair complexes in acidic buffers. After extracting in chloroform, the ion-pair complexes are spectrophotometrically determined at the optimum wavelength. Optimizations of the reaction conditions were carried out. Beer's law was obeyed within the concentration range from 1 to 15 μg/mL. The molar absorptivity, Sandell sensitivity, and detection and quantification limits were also determined. The developed methods were applied successfully for the determination of these drugs in some available commercial preparations. The results were compared statistically with those obtained from reported high-performance liquid chromatography methods.


2014 ◽  
Vol 2014 ◽  
pp. 1-10 ◽  
Author(s):  
Nejal M. Bhatt ◽  
Vijay D. Chavada ◽  
Mallika Sanyal ◽  
Pranav S. Shrivastav

Objective. Three sensitive, selective, and precise spectrophotometric methods based on manipulation of ratio spectra, have been developed and validated for the determination of diclofenac sodium and pantoprazole sodium.Materials and Methods. The first method is based on ratio spectra peak to peak measurement using the amplitudes at 251 and 318 nm; the second method involves the first derivative of the ratio spectra (Δλ=4 nm) using the peak amplitudes at 326.0 nm for diclofenac sodium and 337.0 nm for pantoprazole sodium. The third is the method of mean centering of ratio spectra using the values at 318.0 nm for both the analytes.Results. All the three methods were linear over the concentration range of 2.0–24.0 μg/mL for diclofenac sodium and 2.0–20.0 μg/mL for pantoprazole sodium. The methods were validated according to the ICH guidelines and accuracy, precision, repeatability, and robustness are found to be within the acceptable limit. The results of single factor ANOVA analysis indicated that there is no significant difference among the developed methods.Conclusions. The developed methods provided simple resolution of this binary combination from laboratory mixtures and pharmaceutical preparations and can be conveniently adopted for routine quality control analysis.


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