scholarly journals A Sensitive Spectrophotometric Estimation of Nimodipine in Tablets and Injection Using Phloroglucinol

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Hemavathi N. Deepakumari ◽  
Hosakere D. Revanasiddappa

A rapid, simple, and sensitive spectrophotometric method has been described for the determination of nimodipine in bulk drug, tablets, and injection. The proposed method is based on the diazotization of reduced nimodipine with nitrous acid followed by coupling with phloroglucinol to form colored azo dye and showing absorption maximum () at 410 nm. The formed colored azo dye is stable for about more than 2 h. The method obeyed Beer’s law over the concentration range of 0–25 μg/mL and the corresponding molar absorptivity value is  L/moL/cm. The Sandell sensitivity values limits of detection (LOD) and quantification (LOQ) values have also been reported for the developed method. The accuracy and precision of the method was evaluated on intra- and interday basis; the relative error (%RE) and the relative standard deviation (RSD) were <2.0%. All variables have been optimized and the presented reaction sequence was applied to the analysis of nimodipine in bulk drug, tablets, and injections. The performance of this method was evaluated in terms of Student’s -test and variance ratio -test to find out the significance of proposed method over the reference method.

2001 ◽  
Vol 84 (1) ◽  
pp. 53-58 ◽  
Author(s):  
Murad I H Helaleh ◽  
Takashi Korenaga

Abstract A new simple, sensitive, and selective spectrophotometric method was developed for the determination of nitrite. The method is based on the reaction of nitrite with sulfathiazole in acidic medium to form a diazonium cation, which is subsequently coupled with N-(1-naphthyl)ethylenediamine dihydrochloride to form a highly stable, violet azo dye. The reaction product has an absorption maximum at 546 nm and obeys Beer's law over a nitrite range of 0.054–0.816 μg/mL. The molar absorptivity of the colored compound is 4.61 × 104 L/(mol·cm). The detection limit is 12.1 μg/L. The relative standard deviation is 0.85% for 5 determinations of nitrite at 0.27 μg/mL. The reproducibility and validity of the proposed method are discussed in the present paper. The simplicity of the method is demonstrated by the high stability of the azo-dye product as well as the short time required for its complete formation in a reaction at room temperature without pH control or extra extraction. The sensitivity of the method is shown by the successful determination of nitrite in human saliva and rain water, and of nitrogen dioxide in the atmosphere. The results compare favorably with those obtained by the reference method. The selectivity of the method is indicated by its freedom from most interferences, even at high concentrations of nitrate (500 μg/mL).


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.


2009 ◽  
Vol 15 (2) ◽  
pp. 77-81 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay

Two simple, rapid, reliable and cost-effective methods based on titrimetry in non-aqueous medium are described for the determination of olanzapine in pharmaceuticals. In these methods, the drug dissolved in the glacial acetic acid was titrated with the acetous perchloric acid with visual and potentiometric end point detection, crystal violet being used as the indicator for visual titration. The methods are applicable over 1-15 mg range of olanzapine. The procedures were applied to determine olanzapine in pharmaceutical products and the results were found to be in a good agreement with those obtained by the reference method. Associated pharmaceutical materials did not interfere. The precision results, expressed by inter-day and intra-day relative standard deviation values, were satisfactory, higher than 2%. The accuracy was satisfactory as well. The methods proved to be suitable for the analysis of olanzapine in bulk drug and in tablets. The accuracy and reliability of the methods were further ascertained by recovery studies via a standard addition technique with percent recoveries in the range 97.51-103.7% with a standard deviation of less than 2%.


2002 ◽  
Vol 70 (1) ◽  
pp. 49-55
Author(s):  
Abou-Attia Fekria M. ◽  
Issa Y.M. ◽  
El Reis M.A. ◽  
Aly F.A. ◽  
Abd El- MoetY M.

The formation of the azo-dye using chromotropic acid as a coupling agent was applied to the determination of five sulphonamides. The spectrophotometric studies as well as microanalysis of the studied sulphonamides- chromotropic acid azo dyes revealed the existence of the 1:1 coupling product. The absorbance of the formed azo dye is measured at 510 nrn, and has a large molar absorptivity (ε = 2.87 - 3.29 × 104 1 mol−1cm−1). Beer's law was obeyed over the concentration range 0.5-9.0 µg ml−1. The assay results of pharmaceutical formulations showed good accuracy and precision over the concentration range used. The proposed method avoids time-consumption, extraction process and temperature control.


1990 ◽  
Vol 55 (7) ◽  
pp. 1686-1690 ◽  
Author(s):  
José Aznarez ◽  
Juan Carlos Vidal ◽  
Cecilia Vaquero

A method for tantalum(V) spectrophotometric determination in a non-aqueous phase is proposed. Tantalum(V) is extracted with N-phenylbenzohydroxamic acid into toluene from a 5M hydrochloric acid solution. The colour is then developed by addition of 4-(2-pyridylazo)-resorcinol (PAR) solution in N,N-dimethylformamide and pyridine to an aliquot of the extracted phase. The Ta(V)-PAR complex gives an absorption maximum at 547 nm with a molar absorptivity of 3.88 ± 0.04 . 104 l mol-1 cm-1. The method has been applied to the selective determination of tantalum in ores with good accuracy and precision.


2020 ◽  
Vol 1002 ◽  
pp. 350-359
Author(s):  
Asmaa Ahmed Mohammed Al Rashidy ◽  
Khalid Abdlaaziz Al Badrany ◽  
Gassim Mohammed Al Garagoly

Simple, sensitive and accurate spectrophotometric methods have been developed for the determination of Sulphamethoxazole (SMZ) drug . This method based on the reaction of Sulphamethoxazole (SMZ) with new organic reagent (BYN) it was prepare by reaction between ethyl acetoacetate with 2,4-Dinitrophenylhydrazine. The azo dye product shows absorption maximum at 435 nm. The linearity ranges of Sulphamethoxazole are (2-14 μg.mL-1) with molar absorptivity (14412.77 L.mol-1.cm-1), Sandell's sensitivity index (0.0175 μg.cm-2) , detection limit and Quantification limit ( 0.057, 0.175 μg / ml) respectively. The results showed there are no interferences of excipients on the determination of the drug. The proposed method has been successfully applied for the determination of sulfanilamide in pure and pharmaceutical formulations.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Kudige N. Prashanth ◽  
Kanakapura Basavaiah ◽  
Madihalli S. Raghu

An accurate and precise spectrophotometric method is presented for the determination of zolmitriptan (ZMT) based on the formation of a red color product with vanillin in presence of concentrated H2SO4, with the chromogen being measured at 580 nm. The reaction proceeds quantitatively at room temperature in 10 min. The calibration curve is linear over the range 5.0–90.0 μg mL−1 and described by the regression equation with a regression coefficient of 0.9994 . The calculated molar absorptivity and Sandell sensitivity values are 3.3 × 103 L mol−1 cm−1 and 0.0872 μg cm−2, respectively. The limits of detection (LOD) and quantification (LOQ) calculated as per ICH guidelines are 1.26 and 3.81 μg mL−1, respectively. The within-day accuracy expressed as relative error was better than 1.78% with precision (RSD) ranging from 0.83 to 1.45%. The between-day accuracy ranged from 1.21 to 1.84% with a precision less than 1.66%. The method was successfully applied to the analysis of one brand of tablet containing zolmitriptan. The results obtained were in agreement with those obtained by published reference method. The accuracy was also checked by placebo blank and synthetic mixture analyses besides recovery study via standard addition procedure.


2013 ◽  
Vol 830 ◽  
pp. 298-301 ◽  
Author(s):  
Lin Gao ◽  
Yan Hua Li ◽  
Sheng Jie Chen ◽  
Fang Chen ◽  
Yuan Fang Zhang ◽  
...  

p-Carboxyarsenazo (CASA) color reagent was synthesized by simple diazotization reaction, and the chromomeric reaction between CASA with Cu(Ⅱ) has been studied by spectrophotometry. In pH=4.6 NaAc-HAc buffer solution, Cu(Ⅱ) reacted with CASA to form a red complex and exhibits an absorption maximum at 614 nm, Beer’s law is obeyed for 0-160 μg/L of copper in solution, the apparent molar absorptivity obtained is 1.57×104 L/(mol.cm), and the relative standard deviation (R.S.D.) is 1.6%. The proposed method exhibited high sensitivity and selectivity for Cu(Ⅱ). The results obtained by this method in the determination of environment water samples were accurate, sensitive and repeatable


2010 ◽  
Vol 60 (4) ◽  
pp. 445-454 ◽  
Author(s):  
Pavagada Ramesh ◽  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad

Sensitive and selective spectrophotometric assay of doxycycline hyclate in pharmaceuticals using Folin-Ciocalteu reagentA spectrophotometric method for the determination of doxycycline (DOX) is described. The method is based on the formation of blue colored chromogen due to reduction of tungstate and/or molybdate in Folin-Ciocalteu (F-C) reagent by DOX in alkaline medium. The colored species has an absorption maximum at 770 nm and the system obeys Beer's law over the concentration range 0.75-12.0 μg mL-1DOX. The apparent molar absorptivity is 2.78 × 104L mol-1cm-1. The limit of quantification and detection values are reported to be 0.20 and 0.08 μg mL-1, respectively. Over the linear range applicable, the accuracy and precision of the method were evaluated on intra-day and inter-day basis. The reported mean accuracy value was 101.0 ± 1.7 %, the relative error was ≤ 2.7 % and the relative standard deviation was ≤ 2.5 %. Application of the proposed method to bulk powder and commercial pharmaceutical tablets is also presented. No significant difference was obtained between the results of the proposed method and the official BP method. The procedure described in this paper is simple, rapid, accurate and precise.


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