scholarly journals Bromatomatric assay of gatifloxacin in pharmaceuticals

2008 ◽  
Vol 14 (3) ◽  
pp. 185-190
Author(s):  
Kanakapura Basavaiah ◽  
Urdigere Kumar ◽  
Kalsang Tharpa
Keyword(s):  
Methyl Orange ◽  
Indigo Carmine ◽  
Pharmaceutical Preparations ◽  
Cost Effective ◽  
Thymol Blue ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Hydrochloric Acid Medium ◽  
Ich Guidelines

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.

scholarly journals NOVEL SELECTIVE SPECTROPHOTOMETRIC METHODS FOR THE DETERMINATION OF METHIMAZOLE IN PURE FORM AND IN PHARMACEUTICAL FORMULATION

2019 ◽  
pp. 62-69
Author(s):  
MALAK Y. AL BATHISH ◽  
AZZA A. GAZY ◽  
MARWA K. EL JAMAL
Keyword(s):  
Methyl Orange ◽  
Pharmaceutical Preparations ◽  
Fixed Time ◽  
Pharmaceutical Formulation ◽  
Pure Form ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Resultant Solution

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.

scholarly journals New Sensitive Spectrophotometric Methods for the Determination of Raloxifene Hydrochloride in Pharmaceuticals Using Bromate-Bromide,Methyl Orange and Indigo Carmine

2006 ◽  
Vol 3 (4) ◽  
pp. 242-249 ◽  
Author(s):  
K Basavaiah ◽  
U. R. Anil Kumar
Keyword(s):  
Methyl Orange ◽  
Indigo Carmine ◽  
Reference Method ◽  
Standard Addition ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Hydrochloric Acid Medium ◽  
Student’S T ◽  
Raloxifene Hydrochloride

Two new sensitive spectrophotometric methods are proposed for the determination of raloxifene hydrochloride (RLX) using bromate-bromide mixture and two dyes, methyl orange and indigocarmine, as reagents. The methods entail the addition of a known excess of bromate-bromide mixture to RLX 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). In both methods, the amount of bromine reacted corresponds to the amount of RLX. The absorbance is found to increase linearly with concentration of RLX. Under the optimum conditions, RLX could be assayed in the concentration range 0.1-2.0 and 0.5-6.0 μg mL-1by method A and method B, respectively. The apparent molar absorptivities are calculated to be 1.9×105and 4.5×104L mol-1cm-1for method A and method B, respectively, and the corresponding Sandell sensitivity values are 0.003 and 0.011 μg cm-2. The limits of detection and quantification are also reported for both methods. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The methods were successfully applied to the assay of RLX in its tablet formulation and the results were compared with those of a reference method by calculating the Student’s t-value and F-value. No interference was observed from common tablet adjuvants. The accuracy and reliability of the methods were further ascertained by recovery experiments via standard-addition procedure.

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
Keyword(s):  
Phosphate Buffer ◽  
Pharmaceutical Preparations ◽  
High Sensitivity ◽  
Cost Effective ◽  
Sensitivity Coefficient ◽  
Molar Absorptivity ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Beer’S Law

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 %).

scholarly journals Use of ceric ammonium sulphate and two dyes, methyl orange and indigo carmine, in the determination of lansoprazole in pharmaceuticals

2007 ◽  
Vol 57 (2) ◽  
pp. 211-220 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Veeraiah Ramakrishna ◽  
Urdigere Kumar
Keyword(s):  
Methyl Orange ◽  
Ammonium Sulphate ◽  
Indigo Carmine ◽  
Correlation Coefficients ◽  
Standard Addition ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Bulk Drug

Use of ceric ammonium sulphate and two dyes, methyl orange and indigo carmine, in the determination of lansoprazole in pharmaceuticalsTwo spectrophotometric methods are proposed for the assay of lansoprazole (LPZ) in bulk drug and in dosage forms using ceric ammonium sulphate (CAS) and two dyes, methyl orange and indigo carmine, as reagents. The methods involve addition of a known excess of CAS to LPZ in acid medium, followed by determination of residual CAS by reacting with a fixed amount of either methyl orange, measuring the absorbance at 520 nm (method A), or indigo carmine, measuring the absorbance at 610 nm (method B). In both methods, the amount of CAS reacted corresponds to the amount of LPZ and the measured absorbance was found to increase linearly with the concentration of LPZ, which is corroborated by the correlation coefficients of 0.9979 and 0.9954 for methods A and B, respectively. The systems obey Beer's law for 0.5-7.0 μg mL-1and 0.25-3.0 μg mL-1for methods A and B, respectively. The apparent molar absorptivities were calculated to be 3.0 x 104and 4.4 x 104L mol-1cm-1for methods A and B, respectively. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.08 and 0.25 μg mL-1for method A, and 0.09 and 0.27 μg mLs-1for method B, respectively. The intra-day and inter-day precision and accuracy of the methods were evaluated according to the current ICH guidelines. Both methods were of comparable accuracy (er≤ 2 %). Also, both methods are equally precise as shown by the relative standard deviation values < 1.5%. No interference was observed from common pharmaceutical adjuvants. The accuracy of the methods was further ascertained by performing recovery studies using the standard addition method. The methods were successfully applied to the assay of LPZ in capsule preparations and the results were statistically compared with those of the literature UV-spectrophotometric method by applying Student'st-test andF-test.

scholarly journals Titrimetric and Spectrophotometric Determination of Metaprolol tartrate in Pharmaceuticals Using N-Bromosuccinimide

2007 ◽  
Vol 4 (1) ◽  
pp. 117-127 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar
Keyword(s):  
Methyl Orange ◽  
Indigo Carmine ◽  
Reference Method ◽  
Standard Addition ◽  
Reaction Conditions ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Bulk Drug ◽  
Reaction Stoichiometry

One titrimetric and two spectrophotometric methods are presented for the assay of metaprolol tartrate (MPT) in bulk drug and in tablets. The methods employ N-bromosuccinimide (NBS) as the oxidimetric reagent and two dyes, methyl orange and indigo carmine as spectrophotometric reagents. In titrimetry, an acidified solution of MPT is treated with a known excess amount of NBS and after a definite time, the unreacted oxidant is determined by iodometric back titration. Spectrophotometry involves adding a measured excess of NBS to MPT in acid medium followed by determination of residual NBS 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). In all the methods, the amount of NBS reacted corresponds to the amount of MPT. Reaction conditions have been optimized. Titrimetry allows the determination of 1 - 12 mg of MPT and the calculations are based on a 1: 4 (MPT: NBS) reaction stoichiometry. In spectrophotometry, the measured absorbance is found to increase linearly with the concentration of MPT serving as basis for quantitation. The systems obey Beer’s law for 0.5 - 4.0 μg mL-1and 1.25 - 10.0 μg mL-1for method A and method B, respectively. The apparent absorptivities are calculated to 1.07 × 105be and 4.22 × 104L mol cm-1for method A and method B, respectively. The methods developed were applied to the assay of MPT in commercial tablet formulations, and the results were compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition method.

scholarly journals Simple Spectrophotometric Methods for the Determination of Zidovudine in Pharmaceuticals Using Chloramine-T, Methylene Blue and Rhodamine-B as Reagents

2006 ◽  
Vol 3 (3) ◽  
pp. 173-181
Author(s):  
K. Basavaiah ◽  
U. R. Anil Kumar
Keyword(s):  
Methylene Blue ◽  
Rhodamine B ◽  
Pharmaceutical Formulations ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Hydrochloric Acid Medium ◽  
Ich Guidelines ◽  
Chloramine T ◽  
Bulk Drug

Two new spectrophotometric methods are proposed for the determination of zidovudine(ZDV) in pharmaceuticals. The methods use chloramine-T (CAT) and two dyes, methylene blue and rhodamine-B, as reagents and are based on adding of a known excess of CAT to ZDV in hydrochloric acid medium followed by determination of residual oxidant by reacting with a fixed amount of either methylene blue and measuring the absorbance at 665 nm (Method A) or rhodamine B and measuring the absorbance at 555 nm (Method B). In both methods, the amount of CAT reacted corresponds to the amount of ZDV. The absorbance measured is found to increase linearly with concentration of ZDV. Under the optimum conditions, ZDV could be assayed in the concentration range 1.25-15.0 and 0.25-3.0 μg ML-1by method A and method B, respectively. The apparent molar absorptivities are calculated to be 7.7x103and 5.6x104L mol-1cm-1for method A and method B, respectively, and the corresponding Sandell sensitivity values are 0.035 and 0.005 μg cm-2. The limits of detection and quantification are reported for both methods. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The proposed methods can be readily utilized for bulk drug and in pharmaceutical formulations.

scholarly journals Titrimetric and spectrophotometric determination of doxycycline hyclate using bromate-bromide, methyl orange and indigo carmine

2010 ◽  
Vol 16 (2) ◽  
pp. 139-148 ◽  
Author(s):  
Jagannathamurthy Ramesh ◽  
Kanakapura Basavaiah ◽  
Ranganath Divya ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay
Keyword(s):  
Methyl Orange ◽  
Indigo Carmine ◽  
Molar Absorptivity ◽  
Stoichiometric Ratio ◽  
Doxycycline Hyclate ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Bulk Drug

One titrimetric and two indirect spectrophotometric methods are described for the determination of doxycycline hyclate (DCH) in bulk drug and in its formulations. The methods use bromate-bromide, methyl orange and indigo carmine as reagents. In titrimetry (method A), DCH is treated with a known excess of bromate-bromide mixture in acid medium and the residual bromine is back titrated iodometrically after the reaction between DCH and in situ bromine is ensured to be complete. In spectrophotometric methods, the excess of bromine is estimated by treating with a fixed amount of either methyl orange (method B) or indigo carmine (method C) and measuring the change in absorbance either at 520 or 610 nm. Titrimetric method is applicable over 1-8 mg range and the calculations are based on a 1:2 (DCH:bromate) stoichiometric ratio. In spectrophotometry, the calibration graphs were found to be linear over 0.25-1.25 and 1-5 ?g mL-1 for method B and method C, respectively, with corresponding molar absorptivity values of 2.62 ?105 and 6.97 ? 104 L mol-1 cm-1. Accuracy and precision of the assays were determined by computing the intra-day and inter-day variations at three different levels of DCH.

scholarly journals Sensitive Bromatometric Methods for the Determination of Sumatriptan Succinate in Pharmaceutical Formulations

2011 ◽  
Vol 8 (1) ◽  
pp. 269-275 ◽  
Author(s):  
K. V. V. Satyanarayana ◽  
P. Nageswara Rao
Keyword(s):  
Indigo Carmine ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Sumatriptan Succinate ◽  
Ich Guidelines ◽  
Label Claim

Two simple and sensitive spectrophotometric methods are described for the determination of sumatriptan succinate (STS) in pure and tablets using bromate-bromide as the bromination reagent in acid medium and two dyes as subsidiary reagents. The two methods are based on the bromination of STS by a known excess ofin situgenerated bromine followed by determination of unreacted bromine by reacting with a fixed amount of methyl orange (Method A) or indigo carmine (Method B) and measuring the absorbance at 508 or 610 nm. In both methods, the amount of bromine reacted corresponds to the amount of STS. The experimental conditions for the assay have been optimized. In two methods, the absorbance was found to increase linearly with the concentration of STS at the respective wavelengths. Beer’s law was obeyed over the ranges 0.2-1.6 and 2.0-12.0 μg mL-1for method A and method B respectively and the respective molar absorptivity values were 1.898×105and 2.71×104L mol-1cm-1. The statistical analysis of the methods was validated according to the present ICH guidelines. The proposed methods were applied to the analysis of tablet form of STS and the results tallied well with the label claim.

scholarly journals SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF SOFOSBUVIR AND DACLATASVIR IN PURE AND DOSAGE FORMS

2021 ◽  
pp. 112-119
Author(s):  
MONIR Z. SAAD ◽  
ATEF AMER ◽  
KHALED ELGENDY ◽  
BASEM ELGENDY
Keyword(s):  
Indigo Carmine ◽  
Reference Method ◽  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Fixed Amount ◽  
Alizarin Red ◽  
Spectrophotometric Methods

Objective: Two simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sofosbuvir (SOF) and daclatasvir (DAC) in pure forms and pharmaceutical formulations. Methods: The proposed methods are based on the oxidation of SOF and DAC by a known excess of cerium(IV) ammonium nitrate in sulphuric acid medium followed by determination of unreacted cerium(IV) by adding a fixed amount of indigo carmine (IC) and alizarin red S (ARS) dyes followed by measuring the absorbance at 610 and 360 nm, respectively. The experimental conditions affecting the reaction were studied and optimized. Results: The beer’s law was obeyed in the concentration ranges of 0.2-3.0, 0.2-4.0 for SOF and 0.5-4.5 and 0.5-5.0 μg/ml for DAC using IC and ARS methods, respectively with a correlation coefficient ≥ 0.9991. The calculated molar absorptivity values are 2.354 × 104, 1.933 × 104 for SOF and 1.786 × 104 and 2.015 × 104 L/mol. cm for DAC using IC and ARS methods, respectively u. The limits of detection and quantification are also reported. Intra-day and inter-day precision and accuracy of the methods have been evaluated. Conclusion: The methods were successfully applied to the assay of SOF and DAC in tablets and the results were statistically compared with those of the reference method by applying Student’s t-test and F-test. No interference was observed from the common tablet excipients. The accuracy and reliability of the methods were further ascertained by performing recovery studies using the standard addition method.

scholarly journals Sensitive and rapid titrimetric and spectrophotometric methods for the determination of stavudine in pharmaceuticals using bromate-bromide and three dyes

2008 ◽  
Vol 80 (2) ◽  
pp. 253-262 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Veeraiah Ramakrishna ◽  
Chikkaswamy Somashekar ◽  
Urdigere R. Anil Kumar
Keyword(s):  
Dosage Forms ◽  
Linear Increase ◽  
Thymol Blue ◽  
Fixed Amount ◽  
Rapid Methods ◽  
Spectrophotometric Methods ◽  
Back Titration ◽  
Bulk Drug ◽  
Hcl Medium

Four sensitive and rapid methods for the determination of stavudine (STV) in bulk drug and in dosage forms were developed and optimized. In titrimetry, aqueous solution of STV was treated with a known excess of bromate-bromide in HCl medium followed by estimation of unreacted bromine by iodometric back titration. Spectrophotometric methods involve the addition of a measured excess of bromate-bromide in HCl medium and subsequent estimation of the residual bromine by reacting with a fixed amount of methyl orange, indigocarmine or thymol blue followed by measurement of absorbance at 520 nm (method A), 610 nm (method B) or 550 nm (method C). In all the methods, the amount of bromate reacted corresponds to the amount of STV. Calculations in titrimetry were based on a 1:0.666 (STV:KBrO3) stoichiometry and the method was found to be applicable over 3.5-10 mg range. A linear increase in absorbance with concentration of STV was observed in the spectrophotometric methods, and the Beer's law was obeyed over the concentration ranges 0.125-1.75, 1-10 and 1-9.0 µg mL-1 STV for method A, method B and method C, respectively. The methods when applied to the determination of STV in tablets and capsules were found to give satisfactory results.

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