scholarly journals Condensation Methods for the Determination of Darunavir in Pure and Pharmaceutical Formulations

2020 ◽  
Vol 13 (4) ◽  
pp. 394-401
Author(s):  
M.L.N. Acharyulu ◽  
P.V.S.R. Mohana Rao ◽  
I. Siva Ramakoti
Keyword(s):  
Regression Analysis ◽  
Acidic Medium ◽  
Low Cost ◽  
Condensation Reaction ◽  
Reference Method ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Spectrophotometric Methods

Two visible spectrophotometric methods were developed Aand B for the determination of Darunavir in pure and pharmaceutical formulations. The methods are based on condensation reaction with PDAB (Method-A) and ONB (Method-B) in presence of acidic medium with the primaryamine group in DNV. The coloured products exhibit absorption λmax at 639 nm and 452nm for methods A and B respectively. Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 10-60μg/ml, 50-300 μg/ml, correlation co-efficients are 0.9983, 0.9989;Sandell’s sensitivities are9.9833 x 10-3, 3.0456 x 10-2(1 mole cm-1); and molar absorptivity values are5.4857 x 104,1.7981x 104 (μg cm-2) for methods-Aand B respectively. The proposed methods are applied to commercial available formulations and the results are statistically compared with those obtained by the UV reference method and validated by recovery studies. The results are found satisfactory and reproducible. These methods are applied successfully for the estimation of the DNV in the presence of other ingredients that are usually present in formulations. These methods offer the advantages of rapidity, simplicity and sensitivity and low cost without the need for expensive instrumentation and reagents.

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 New Spectrophotometric Methods for Estimation of Perindopril Erbumine in Bulk and Pharmaceutical Formulations

2014 ◽  
Vol 6 (2) ◽  
pp. 319-327
Author(s):  
A. Unnisa ◽  
K. V. G. Raju ◽  
K. Balaji ◽  
A. N. Jyothi ◽  
T. S. Kumar
Keyword(s):  
Regression Analysis ◽  
Citric Acid ◽  
Pharmaceutical Formulations ◽  
Bulk Sample ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Spectrophotometric Methods ◽  
Perindopril Erbumine ◽  
Detection And Quantification

Three rapid, simple, inexpensive, precise, and accurate spectrophotometric procedures were developed for the determination of Perindopril erbumine (PPE) using cobalt-thiocyanate, citric acid and 2,3- dichloro-5,6-dicyano benzoquinone in bulk sample and in dosage forms. The procedures are based on the coordination complex of the drug (electron donor) and the chromogenic reagents used. The colored products are extracted into non aqueous solvents and measured spectrophotometrically at the optimum ?maxfor each complex. Regression analysis of Beer-Lambert plots showed good correlation in the concentration range of 30-70 µg mL?1, 4-20 µg mL?1 and 20-60 µg mL?1 for cobalt-thiocyanate, citric acid and 2,3- dichloro-5,6-dicyano benzoquinone, respectively. The apparent molar absorptivity, Sandell’s sensitivity, detection and quantification limits were calculated. The developed methods were successfully applied for the determination of PPE in bulk and pharmaceutical formulations without any interference from common excipients and hence can be used for their routine analysis. Keywords: Perindopril erbumine; Spectrophotometry; Cobalt-thiocyanate; Citricacid-acetic anhydride.  © 2014 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.   doi: http://dx.doi.org/10.3329/jsr.v6i2.16106 J. Sci. Res. 6 (2), 319-327 (2014)

scholarly journals Spectrophotometric Methods for the Assay of Fluvoxamine Using Chromogenic Reagents

2010 ◽  
Vol 7 (4) ◽  
pp. 1539-1545
Author(s):  
V. Annapurna ◽  
G. Jyothi ◽  
V. Nagalakshmi ◽  
B. B. V. Sailaja
Keyword(s):  
Ascorbic Acid ◽  
Regression Analysis ◽  
Standard Error ◽  
Oxidative Coupling ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Method Of Least Squares ◽  
Spectrophotometric Methods ◽  
Uv Visible

Simple, accurate and reproducible UV-Visible spectrophotometric methods were established for the assay of FXA based on the oxidative coupling and condensation reactions. Condensation and coupling of the FXA with Ninhydrin-Ascorbic acid is proposed in method A. Method B includes complexation of FXA with cobalt thiocyanate. The ligating property of FXA with sodium nitro prusside is incorporated in method C. The optical characteristics such as Beers law limits, molar absorptivity and Sandell’s sensitivity for the methods (A-C) are given. Regression analysis using the method of least squares was made to evaluate the slope(b), intercept(a) and correlation coefficient (r) and standard error of estimation (Se) for each system. Determination of FXA in bulk form and in pharmaceutical formulations were also incorporated.

scholarly journals Indirect spectrophotometric determination of diltiazem hydrochloride in pure form and pharmaceutical formulations

2005 ◽  
Vol 3 (3) ◽  
pp. 520-536 ◽  
Author(s):  
Akram El-Didamony
Keyword(s):  
Reference Method ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Pure Form ◽  
Diltiazem Hydrochloride ◽  
Spectrophotometric Methods ◽  
Chromotrope 2R ◽  
Significant Difference ◽  
Comparison Of The Results

AbstractThree simple, accurate, and sensitive spectrophotometric methods (A, B and C) have been described for the indirect assay of diltiazem hydrochloride (DIL.HCl), either in pure form or in pharmaceutical formulations. The first method (A) is based on the oxidation of DIL.HCl by N-bromosuccinimide (NBS) and determination of unconsumed NBS by measuring the decrease in absorbance of amaranth dye (AM) at a suitable λmax=521 nm. Other methods (B) and (C) involve the addition of excess cerric ammonium sulfate (CAS) and subsequent determination of the unconsumed oxidant by a decrease in the red color of chromotrope 2R (C2R) at a suitable λmax=528 nm or a decrease in the orange-pink color of rhodamine 6G (Rh6G) at λmax=525 nm, respectively. Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 3.0–9.0, 3.5–7.0 and 3.5–6.3 μg ml−1 for methods A, B and C, respectively. The apparent molar absorptivity, Sandell's sensitivity, detection and quantification limits were calculated. The proposed methods have been applied successfully for the analysis of the drug in its pure form and its dosage form. No interference was observed from a common pharmaceutical adjuvant. Statistical comparison of the results with the reference method shows excellent agreement and indicates no significant difference in accuracy and precision.

scholarly journals Spectrophotometric Determination of Reboxetine through Condensation and Diazo-Coupling Reactions

2011 ◽  
Vol 8 (1) ◽  
pp. 281-287 ◽  
Author(s):  
K. Srikanth ◽  
K. A. Emmanuel
Keyword(s):  
Condensation Reaction ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Good Precision ◽  
Coupling Reactions ◽  
Spectrophotometric Methods ◽  
Methane Sulphonate ◽  
Diazo Coupling ◽  
Hydrolysis Of

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.

scholarly journals Application of bromate-bromide mixture as a green brominating agent for the spectrophotometric determination of atenolol in pharmaceuticals

2012 ◽  
Vol 18 (1) ◽  
pp. 43-52 ◽  
Author(s):  
Nagaraj Prashanth ◽  
Kanakapura Basavaiah ◽  
Sameer Abdulrahman ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay
Keyword(s):  
Reference Method ◽  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Spectrophotometric Methods ◽  
Highly Sensitive ◽  
Bromination Reaction ◽  
Excess Iodide ◽  
Good Agreement

Two highly sensitive spectrophotometric methods are proposed for the quantification of atenolol (ATN) in pure drug as well as in pharmaceutical formulations. The methods are based on the bromination reaction of ATN with a known excess of bromate-bromide mixture in acid medium followed by the determination of unreacted bromine. The residual bromine is determined by its reaction with excess iodide and the liberated iodine (I3?) is either measured at 360 nm (method A) or reacted with starch followed by the measurement of the starch-iodine chromogen at 570 nm (method B). Under the optimum conditions, ATN could be assayed in the concentration ranges of 0.5-9.0 and 0.3-6.0?g mL-1 for method A and method B, respectively, with corresponding molar absorptivity values of 2.36?104 and 2.89?104 L/mol.cm. Sandell?s sensitivity values are found to be 0.0113 and 0.0092 ?g/cm2 for method A and method B, respectively. The proposed methods were successfully applied to the analysis of different commercial brands of pharmaceutical formulations and the results obtained by the proposed methods were in good agreement with those obtained using the reference method. The reliability of the methods was further ascertained by recovery studies using standard- addition method.

scholarly journals Spectrophotometric Determination of Gemifloxacin Mesylate in Pharmaceutical Formulations Through Ion-Pair Complex Formation

2008 ◽  
Vol 5 (3) ◽  
pp. 515-520 ◽  
Author(s):  
Marothu Vamsi Krishna ◽  
Dannana Gowri Sankar
Keyword(s):  
Methylene Blue ◽  
Acidic Medium ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Basic Medium ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Safranin O

Four simple and sensitive ion-pairing spectrophotometric methods have been described for the assay of gemifloxacin mesylate (GFX) either in pure form or in pharmaceutical formulations. The developed methods involve formation of colored chloroform extractable ion-pair complexes of the drug with safranin O (SFN O) and methylene blue (MB) in basic medium; Napthol blue 12BR (NB 12BR) and azocaramine G (AG) in acidic medium. The extracted complexes showed absorbance maxima at 525, 650, 620 and 540 nm for SFN O, MB, NB 12BR and AG, respectively.Beer's law is obeyed in the concentration ranges 3-15, 4-20, 2-10 and 2-10 μg/mL with molar absorptivity of 2.81 × 104, 2.20 x 104, 4.02 × 104and 4.15 × 104L mole−1cm−1and relative standard deviation of 0.077, 0.104, 0.080 and 0.103% for SFN O, MB, NB 12BR and AG, respectively. These methods have been successfully applied for the assay of drug in pharmaceutical formulations. No interference was observed from common pharmaceutical adjuvants. Results of analysis were validated statistically and through recovery studies.

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 the Assay of Pyrilamine Maleate Using Chromogenic Reagents

2010 ◽  
Vol 7 (4) ◽  
pp. 1507-1513 ◽  
Author(s):  
V. Annapurna ◽  
G. Jyothi ◽  
V. Nagalakshmi ◽  
B. B. V. Sailaja
Keyword(s):  
Charge Transfer ◽  
Oxidative Coupling ◽  
Coupling Reaction ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Method Of Least Squares ◽  
Spectrophotometric Methods ◽  
Oxidative Coupling Reaction ◽  
Charge Transfer Complexation

Simple, accurate and reproducible UV spectrophotometric methods were established for the assay of pyrilamine maleate (PYRA) based on the formation of oxidative coupling and precipitation, charge transfer complexation products. Method A includes the oxidative coupling reaction of PYRA with 3-methyl-2-benzathiazolinone hydrazone (MBTH) in presence of Ce(IV). The formation of oxidative coupling product with 4-amino phenazone (4-AP) in presence of K3Fe(CN)6is incorporated in method B. Precipitation/charge transfer complex formation of the PYRA with tannic acid (TA)/Metol-Cr(VI) in method C were proposed. The optical characteristics such as Beers law limits, molar absorptivity and Sandell’s sensitivity for the methods (A-C) are given. Regression analysis using the method of least squares was made to evaluate the slope (b), intercept (a) and correlation coefficient (r) and standard error of estimation (Se) for each system. Determination of pyrilamine in bulk form and in pharmaceutical formulations were also incorporated.

scholarly journals Sensitive Spectrophotometric Methods for the Determination of Ascorbic Acid

2008 ◽  
Vol 5 (1) ◽  
pp. 10-15 ◽  
Author(s):  
H. D. Revanasiddappa ◽  
M. A. Veena
Keyword(s):  
Ascorbic Acid ◽  
Acid Medium ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Spectrophotometric Methods ◽  
Maximum Absorbance ◽  
Hydrochloric Acid Medium ◽  
Subsequent Determination ◽  
Sulphuric Acid Medium

Two simple and sensitive spectrophotometric methods (A and B) have been described for the determination of ascorbic acid. Method A is based on the oxidation of ascorbic acid (AA) by known excess of Se(IV) in hydrochloric acid medium and subsequent determination of unreacted Se(IV) by reacting it with iodide in the same acid medium to liberate iodine, which react with starch to form a stable blue coloured iodine-starch complex, which shows maximum absorbance at 590 nm. Method B is based on the oxidation of ascorbic acid (AA) by known excess of Cr(VI) in sulphuric acid medium and the determination of unreacted Cr(VI) with diphenyl carbazide (DPC) under the same acidic medium to produce a stable red-violet coloured species, which shows a maximum absorbance at 550 nm. The reacted oxidants (in methods A and B) correspond to the AA content. The apparent molar absorptivity values are found to be 1.627×104and 1.641×104L mol-1cm-1for methods A and B, respectively. The proposed methods are simple, sensitive and suitable for the routine analysis of AA in pharmaceutical formulations and in real samples.

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