scholarly journals Titrimetric and Spectrophotometric Assay of Pantoprazole in Pharmaceuticals Using Permanganate

2019 ◽  
Vol 53 (1) ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad ◽  
Kalsang Tharpa ◽  
Urdigere Rangachar Anilkumar ◽  
Salamara Ganeshbhat Hiriyanna ◽  
...  
Keyword(s):  
Standard Addition ◽  
Molar Absorptivity ◽  
Calibration Graph ◽  
Spectrophotometric Assay ◽  
Experimental Conditions ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Sensitivity And Selectivity ◽  
Reaction Stoichiometry

Titrimetric and spectrophotometric assay of pantoprazole sodium (PPS) using permanganate as the oxidimetric reagent is described. In titrimetry, PPS is treated with a measured excess of permanganate in H2SO4 medium followed by the determination of unreacted oxidant by back titrating with a standard iron(II) solution. Spectrophotometry involves addition of a known excess of permanganate to PPS in H2SO4 medium followed by the measurement of absorbance of the residual permanganate at 545 nm. In both the methods, the amount of permanganate reacted corresponds to the PPS content. Experimental conditions that provide wide linear range, maximum sensitivity and selectivity, and accuracy and precisions have been optimized. In titrimetry, the calculations are based on a 1:1 (PPS : KMnO4) reaction stoichiometry and the method is applicable over 1.0-7.0 mg range. In spectrophotometry, Beer’s law is obeyed over the concentration range 15.0-150.0 µg mL-1. The linear regression equation of the calibration graph is A = 0.78 + 0.005 C with a regression coefficient (r) of 0.9982 (n = 11). The apparent molar absorptivity is calculated to be 2.213 × 103 l mol-1cm-1 and the Sandell sensitivity is 0.1954 µg cm-2. The limits of detection (LOD) and quantification (LOQ) calculated as per the ICH guidelines are 0.73 and 2.21 µg mL-1, respectively. Accuracy and precision of the assays were determined by computing the intra-day and inter-day variations at three different levels of PPS; the intra-day and inter-day RSD was < 3.09 % and the accuracy was better than 3.5 %. The methods were successfully applied to the determination of PPS in three different brands of tablets with good accuracy and precision, and without detectable interference by excipients. The accuracy was further ascertained by placebo blank and synthetic mixture analyses and also by recovery experiments via standard-addition procedure.

scholarly journals Titrimetric and spectrophotometric assay of diethylcarbamazine citrate in formulations using iodate and iodide mixture as reagents

2015 ◽  
Vol 51 (1) ◽  
pp. 43-52 ◽  
Author(s):  
Nagaraju Swamy ◽  
Kudige Nagaraj Prashanth ◽  
Kanakapura Basavaiah
Keyword(s):  
Molar Absorptivity ◽  
Potassium Iodate ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Diethylcarbamazine Citrate ◽  
Back Titration ◽  
Bulk Drug ◽  
Reaction Stoichiometry

One titrimetric and two spectrophotometric methods are proposed for the determination of diethylcarbamazine citrate (DEC) in bulk drug and in formulations using potassium iodate and potassium iodide as reagent. The methods employ the well-known analytical reaction between iodate and iodide in the presence of acid. In titrimetry (method A), the drug was treated with a measured excess of thiosulfate in the presence of unmeasured excess of iodate-iodide mixture and after a standing time of 10 min, the surplus thiosulfate was determined by back titration with iodine towards starch end point. Titrimetric assay is based on a 1:3 reaction stoichiometry between DEC and iodine and the method is applicable over 2.0-10.0 mg range. The liberated iodine is measured spectrophotometrically at 370 nm (method B) or the iodine-starch complex measured at 570 nm (method C). In both methods, the absorbance is found to be linearly dependent on the concentration of iodine, which in turn is related to DEC concentration. The calibration curves are linear over 2.5-50 and 2.5-30 µg mL-1 DEC for method B and method C, respectively. The calculated molar absorptivity and Sandell sensitivity values were 6.48×103 L mol-1 cm-1 and 0.0604 µg cm-2, respectively, for method B, and their respective values for method C are 9.96×103 L mol-1 cm-1 and 0.0393 µg cm-2. The intra-day and inter-day accuracy and precision studies were carried out according to the ICH guidelines. The methods were successfully applied to the analysis of DEC formulations.

scholarly journals Sensitive and selective spectrophotometric determination of pantoprazole sodium in pharmaceuticals using permanganate

2010 ◽  
Vol 16 (1) ◽  
pp. 97-102 ◽  
Author(s):  
Zenita Devi ◽  
K. Basavaiah ◽  
K.B. Vinay
Keyword(s):  
Reference Method ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Calibration Graph ◽  
Neutral Medium ◽  
Experimental Conditions ◽  
Colored Product ◽  
Tablet Dosage ◽  
Better Than

A simple visible spectrophotometric method is described for the determination of pantoprazole sodium sesquihydrate (PSS). The method is based on the formation of a brown colored product on treating PSS with permanganate in neutral medium, the absorbance being measured at 350 nm. The experimental conditions for the assay were optimized. The absorbance is found to increase linearly with the concentration of PSS and the calibration graph is linear in the range of 2.5-40.0 ?g ml-1 with a linear regression coefficient of 0.998. The calculated molar absorptivity value is 1.27?104 l mol-1 cm-1 and the corresponding Sandel sensitivity is 0.0341 ?g cm-2. The limits of detection (LOD) and quantification (LOQ) are calculated to be 0.49 and 1.47 ?g ml-1, respectively. Intra-day and inter-day accuracy expressed as relative error were better than 2.0% and the corresponding precision (RSD) was less than 2.5 %. The developed and validated method was applied to the determination of the active ingredient in a tablet dosage form and the results obtained agreed well with those of the reference method. The accuracy and reliability of the method were ascertained by performing recovery experiments via standard-addition procedure.

scholarly journals Cerimetric determination of simvastatin in pharmaceuticals based on redox and complex formation reactions

2018 ◽  
Vol 33 (2) ◽  
pp. 21
Author(s):  
Kanakapura Basavaiah ◽  
Okram Zenita Devi
Keyword(s):  
Limit Of Detection ◽  
Reference Method ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Spectrophotometric Methods ◽  
Fixed Quantity ◽  
Bulk Drug ◽  
Student’S T

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.

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 Nitroso-R-salt as a sensitive spectrophotometric reagent for the determination of paracetamol in pharmaceutical preparations

2009 ◽  
Vol 6 (3) ◽  
pp. 570-577
Author(s):  
Baghdad Science Journal
Keyword(s):  
Aqueous Solution ◽  
Statistical Difference ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Calibration Graph ◽  
Subsequent Reaction ◽  
Experimental Conditions ◽  
Colored Complex ◽  
British Pharmacopoeia

Nitroso-R-salt is proposed as a sensitive spectrophotometric reagent for the determination of paracetamol in aqueous solution. The method is based on the reaction of paracetamol with iron(III) and subsequent reaction with nitroso-R-salt to yield a green colored complex with maximum absorption at 720 nm. Optimization of the experimental conditions was described. The calibration graph was linear in the concentration range of 0.1 – 2.0 ?g mL-1 paracetamol with a molar absorptivity of 6.9 × 104 L mol-1 cm-1. The method was successfully applied to the determination of paracetamol in pharmaceutical preparations without any interference from common excipients. The method has been statistically evaluated with British Pharmacopoeia method and no statistical difference between methods was found at the 95% confidence level.

scholarly journals Titrimetric and Spectrophotometric Assay of Ganciclovir in Pharmaceuticals Using Cerium(IV) Sulphate as the Oxidimetric Agent

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Pavagada J. Ramesh ◽  
Kanakapura Basavaiah ◽  
Cijo M. Xavier ◽  
Kudige N. Prashanth ◽  
Madihalli S. Raghu ◽  
...  
Keyword(s):  
Acid Medium ◽  
Statistical Treatment ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Calibration Graph ◽  
Spectrophotometric Assay ◽  
Ferrous Ammonium ◽  
Sulphuric Acid Medium ◽  
Reaction Schemes

Titrimetric and spectrophotometric assay of ganciclovir (GNC) is described using cerium(IV) sulphate as the oxidimetric reagent. The methods are based on the oxidation of GNC with a measured excess of cerium(IV) sulphate in acid medium followed by determination of the unreacted oxidant by two different reaction schemes. In titrimetry, the unreacted oxidant was determined by back titration with ferrous ammonium sulphate (FAS) in sulphuric acid medium, and spectrophotometry involves the reaction of residual cerium(IV) with p-DMAB to form brownish-coloured p-dimethylamino quinoneimine whose absorbance was measured at 460 nm. In both methods, the amount of cerium(IV) sulphate reacted corresponds to GNC concentration. Titrimetry is applicable over 3–10 mg range where as, in spcetrophotometry, the calibration graph is linear over the range of 2–10 μg mL−1 and the calculated molar absorptivity value is  L mol−1 cm−1. The validity of the proposed methods was tested by analyzing pure and dosage forms containing GNC. Statistical treatment of the results reflects that the proposed procedures are precise, accurate, and easily applicable for the determination of GNC pure form and in pharmaceutical formulations.

scholarly journals Spectrophotometric Determination of Zolmitriptan in Bulk Drug and Pharmaceuticals Using Vanillin as a Reagent

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Kudige N. Prashanth ◽  
Kanakapura Basavaiah ◽  
Madihalli S. Raghu
Keyword(s):  
Reference Method ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Ich Guidelines ◽  
Red Color ◽  
Reaction Proceeds ◽  
Recovery Study ◽  
Bulk Drug ◽  
Better Than

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.

scholarly journals Sensitive and selective spectrophotometric assay of doxycycline hyclate in pharmaceuticals using Folin-Ciocalteu reagent

2010 ◽  
Vol 60 (4) ◽  
pp. 445-454 ◽  
Author(s):  
Pavagada Ramesh ◽  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad
Keyword(s):  
Molar Absorptivity ◽  
Spectrophotometric Assay ◽  
Doxycycline Hyclate ◽  
Limit Of Quantification ◽  
Pharmaceutical Tablets ◽  
Bulk Powder ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

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.

scholarly journals Redox-Reaction Based Spectrophotometric Assay of Isoniazid in Pharmaceuticals

2014 ◽  
Vol 2014 ◽  
pp. 1-11 ◽  
Author(s):  
N. Swamy ◽  
K. N. Prashanth ◽  
K. Basavaiah
Keyword(s):  
Prussian Blue ◽  
Redox Reaction ◽  
Molar Absorptivity ◽  
Spectrophotometric Assay ◽  
Commercial Formulation ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Beer's Law ◽  
Beer’S Law

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.

scholarly journals Sensitive and Selective Spectrophotometric Determination of Gabapentin in Capsules Using Two Nitrophenols as Chromogenic Agents

2011 ◽  
Vol 2011 ◽  
pp. 1-9 ◽  
Author(s):  
Sameer A. M. Abdulrahman ◽  
Kanakapura Basavaiah
Keyword(s):  
Picric Acid ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Lewis Base ◽  
Pure Form ◽  
Experimental Conditions ◽  
Spectrophotometric Methods ◽  
Significant Difference

Two simple and selective spectrophotometric methods have been proposed for the determination of gabapentin (GBP) in pure form and in capsules. Both methods are based on the proton transfer from the Lewis acid such as 2,4,6-trinitrophenol (picric acid; PA) or 2,4-dinitrophenol (2,4-DNP) to the primary amino group of GBP which works as Lewis base and formation of yellow ion-pair complexes. The ion-pair complexes formed show absorption maximum at 415 and 420 nm for PA and 2,4-DNP, respectively. Under the optimized experimental conditions, Beer's law is obeyed over the concentration ranges of 1.25–15.0 and 2.0–18.0 μg mL−1GBP for PA and 2,4-DNP methods, respectively. The molar absorptivity, Sandell's sensitivity, detection and, quantification limits for both methods are also reported. The proposed methods were applied successfully to the determination of GBP in pure form and commercial capsules. Statistical comparison of the results was performed using Student'st-test and F-ratio at 95% confidence level, and there was no significant difference between the reference and proposed methods with regard to accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition technique.

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