scholarly journals Titrimetric and sensitive spectrophotometric methods for the assay of quetiapine fumarate in pharmaceutical formulations

2011 ◽  
Vol 17 (1) ◽  
pp. 99-106
Author(s):  
Basavaiah Vinay ◽  
Oddarevanna Revanasiddappa ◽  
Jagannathamurthy Ramesh ◽  
Nagaraju Rajendraprasad
Keyword(s):  
Acetic Acid ◽  
Perchloric Acid ◽  
Pharmaceutical Formulations ◽  
Developed Countries ◽  
Calibration Graph ◽  
Quetiapine Fumarate ◽  
Titrimetric Method ◽  
Accuracy And Precision ◽  
Relative Standard

Quetiapine fumarate (QTF) is a selective monoaminergic antagonist with high affinity for the serotonin Type 2 (5HT2), and dopamine type 2 (D2) receptors. Titrimetric and spectrophotometric assay of quetiapine fumarate (QTF) using perchloric acid and acetic acid as reagents are described. The first method (method A) is a non-aqueous titrimetric method and is based on the titration of QTF in glacial acetic acid with 0.01M acetous perchloric acid using crystal violet as indicator. In the second method (method B), QTF has been measured in 0.1M acetic acid spectrophotometrically at a wavelength of 222 nm. The titrimetric method was applicable over the range of 2.0 - 20.0 mg of QTF. The reaction stoichiometry of 1:3 is obtained which served as the basis for calculation. In spectrophotometry, Beer?s law was obeyed over the concentration range of 1.25 - 15.0 ?g mL-1. The linear regression equation of the calibration graph was A = 0.0115 + 0.0673 C with a regression coefficient (r) of 0.9986 (n=7). The apparent molar absorptivity was calculated to be 4.25 ? 104 L mol-1cm-1 and the Sandell sensitivity was 0.0145 ?g cm-2. The limits of detection (LOD) and quantification (LOQ) calculated as per the ICH guidelines were 0.07 and 0.21 ?g 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 QTF. The intra-day and inter-day relative standard deviation (%RSD) were in the range of 0.99 - 2.88 and 1.65 - 2.32%, for method A and method B, respectively, with an acceptable percentage relative error (%RE) < 2%. The methods were successfully applied in the determination of QTF in two different brands of tablets with good accuracy and precision and without detectable interference by excipients. The methods have demonstrated to be simple and easy to apply in routine usage and do not need any costly instrumentation. Therefore, the reported procedures are advantageous and can be adopted in routine quality control laboratories in the developing or under developed countries.

scholarly journals Flow-injection spectrophotometric determination of dipyrone in pharmaceutical formulations using a solid-phase reactor with copper(II) phosphate

2013 ◽  
Vol 11 (11) ◽  
pp. 1830-1836 ◽  
Author(s):  
Viviane Bonifácio ◽  
Orlando Filho ◽  
Luiz Marcolino-Júnior
Keyword(s):  
Flow Injection ◽  
Solid Phase ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Deionized Water ◽  
Alizarin Red ◽  
Relative Standard ◽  
Solid Phase Reactor ◽  
Carrier Stream ◽  
Continuous Use

AbstractIn this work, a flow-injection spectrophotometric method for dipyrone determination in pharmaceutical formulations was developed. Dipyrone sample solutions were injected into a carrier stream of deionized water and the reaction was carried out in a solid-phase reactor (12 cm, 2.0 mm i.d.) packed with Cu3(PO4)2(s) entrapped in a matrix of polyester resin. The Cu(II) ions were released from the solid phase reactor by the formation of Cu(II)-(dipyrone)n complex. When the complex is released, it reacts with 0.02% m/v alizarin red S in deionized water to produce a Cu(VABO3)3 complex whose absorbance was monitored at 540 nm. The calibration graph was linear over the range 5.0×10−5–4.0×10−4 mol L−1 with a detection limit of 2.0×10−5 mol L−1 and relative standard deviation for 10 successive determinations of 1.5% (2.0×10−4 mol L−1 dipyrone solution). The calculated sample throughput was 60 h−1. The column was stable for at least 8 h of continuous use (500 injections) at 25°C. Pharmaceutical formulations were analyzed and the results from an official procedure measurement were compared with those from the proposed FIA method in order to validate the latter method.

scholarly journals Extractive Spectrophotometric Determination of Nortriptyline Hydrochloride Using Sudan II, IV and Black B

2001 ◽  
Vol 69 (2) ◽  
pp. 151-160
Author(s):  
A. Amin ◽  
H. Saleh
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Calibration Graph ◽  
Official Method ◽  
Spectrophotometric Methods ◽  
Sudan Black B ◽  
Relative Standard ◽  
Nortriptyline Hydrochloride

A simple spectrophotometric methods has been developed for the determination of nortriptyline hydrochloride in pure and in pharmaceutical formulations based on the formation of ion-pair complexes with sudun II (SII), sudan (IV) (SIV) and sudan black B (SBB). The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for SII, SIV and SBB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 – 31.0 μg ml−1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml−1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using SII, SIV, and SBB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.

scholarly journals Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals The simultaneous spectrophotometric determination of trimazolin and phenylephrine hydrochloride in nasal preparations

2008 ◽  
Vol 14 (4) ◽  
pp. 261-264 ◽  
Author(s):  
Ivana Savic ◽  
Goran Nikolic ◽  
Ivan Savic ◽  
Vladimir Bankovic
Keyword(s):  
Spectrophotometric Determination ◽  
Pharmaceutical Formulations ◽  
Active Components ◽  
Phenylephrine Hydrochloride ◽  
Drug Substances ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Relative Standard ◽  
High Degree

This paper presents the experimental results for the simultaneous spectrophotometric determination of two active components in nasal solutions. The resolution of two-component mixtures of timazolin and phenylephrine has been accomplished by using partial least-squares. The method comprised of the absorptivity measurement in a nasal solution at wavelengths of 265 and 272 nm, respectively. Notwithstanding the presence of two components and their high degree of spectral overlap, they have been determined simultaneously with high accuracy and precision, with no interference, rapidly and without resorting to extraction procedures using non aqueous solvents. This method was tested and validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation <2 %), while being simple, cheap and less time consuming. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

scholarly journals Implementation of Quality by Design for the Development and Validation of Pioglitazone Hydrochloride by RP-UPLC with Application to Formulated Forms

2012 ◽  
Vol 2012 ◽  
pp. 1-11 ◽  
Author(s):  
Cijo M. Xavier ◽  
Kanakapura Basavaiah
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Process Understanding ◽  
Validation Criteria ◽  
Relative Standard ◽  
Level Of Knowledge ◽  
Bulk Drug ◽  
Development And Validation

Quality by Design (QbD) is a philosophy that refines the level of knowledge associated with a product that uses process understanding to deliver a product with the desired critical quality attributes. The objective of this study was to develop an integrated multivariate QbD approach to develop and quantify the constituent concentrations of pioglitazone hydrochloride (PGZ) drug in its pure and formulated forms. To facilitate studies investigating the determination of PGZ in bulk drug and its pharmaceutical formulations, a rapid UPLC method was developed and validated for the determination of PGZ accompanied by its degradation studies in different stress conditions. The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.01 and 0.05 μg mL−1, respectively. The percent relative standard deviations for robustness and ruggedness were observed within the range of 0.1–1.74. The calibration graph was linear in the range of 0.05–300 μg mL−1. The applicability of the method was shown by analysis of formulated drug samples and spiked human urine. The proposed method can be used for routine analysis in quality controlled laboratories for its bulk and formulated product and this is the first reported UPLC method for the assay of PGZ.

scholarly journals DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR QUANTIFICATION OF ACETIC ACID CONTENT IN AMLODIPINE BESYLATE

2019 ◽  
pp. 8-11
Author(s):  
Sk Manirul Haque ◽  
Ayman Ahmad
Keyword(s):  
Acetic Acid ◽  
Sodium Hydroxide ◽  
Acid Content ◽  
Amlodipine Besylate ◽  
Strong Base ◽  
Titrimetric Method ◽  
Acetic Acid Content ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: To develop and validate a simple and accurate cost-effective titrimetric method according to International Conference Harmonization (ICH) guidelines for acetic acid content in Amlodipine Besylate. Methods: The titration based on general acid-base reaction to form water and salt. Sodium hydroxide act as a strong base and titrated against weak acid (acetic acid). Phenolphthalein used as an indicator and colorless to pink is the endpoint. Sodium hydroxide is standardized with primary standard potassium hydrogen phthalate. Results: The method was linear in the range of 0.75 to 30.25 μg/ml with a correlation coefficient 0.9999. Limit of detection (LOD) and limit of quantitation (LOQ) value were found to be 0.61 and 1.85 μg/ml, respectively. The percentage recovery (98.20–99.97%) and percentage relative standard deviation (%RSD) is less than 2% within the acceptable limit of ICH guidelines. The robustness and ruggedness results were excellent. Method is accurate and precise, no interference from excipients. Conclusion: A new analytical titrimetric method was developed and validated as per ICH guidelines for the determination of acetic acid content in amlodipine. This proposed method applied for routine analysis of acetic acid content in bulk and pharmaceutical formulations of amlodipine besylate.

scholarly journals Determination of Phenylephrine Hydrochloride by Flow Injection Analysis with Chemiluminescence Detection

2001 ◽  
Vol 84 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Yolanda Fuster Mestre ◽  
Luis Lahuerta Zamora ◽  
José Martínez Calatayud
Keyword(s):  
Flow Injection ◽  
Flow Injection Analysis ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Chemiluminescence Detection ◽  
Phenylephrine Hydrochloride ◽  
Sulfuric Acid Medium ◽  
Sample Throughput ◽  
Relative Standard

Abstract A new method is proposed for the determination of phenylephrine hydrochloride by flow injection analysis with direct chemiluminescence detection. The method is based on the oxidation of the drug by potassium permanganate in sulfuric acid medium at 80°C. The calibration graph is linear over the range 0.03–8 ppm phenylephrine hydrochloride, with a relative standard deviation (n = 51, 0.5 ppm) of 1.1% and sample throughput of 134/h. The influence of 38 different foreign compounds was tested, and the method was applied to the determination of phenylephrine hydrochloride in 8 different pharmaceutical formulations.

scholarly journals Kinetics Spectrophotometric determination of Ranitidine based on its Inhibitory effect on the Oxidation Rate of Malachite green by N-bromosuccinide

2020 ◽  
Vol 13 (1) ◽  
pp. 253-261
Author(s):  
Ashraf M. Taha ◽  
Alaa Eldin Mokhtar Abdel-Hady
Keyword(s):  
Malachite Green ◽  
Inhibitory Effect ◽  
Calibration Graph ◽  
Rate Of Change ◽  
Linear Calibration ◽  
Inhibiting Effect ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Kinetic Spectrophotometric

A simple and sensitive kinetic spectrophotometric method is described for the determination of ranitidine. The method is based on the inhibiting effect of ranitidine on the rate of oxidation of malachite green (MG+ ) with N-bromosuccinimide (NBS) The oxidation reaction was followed spectrophotometrically by measuring the rate of change of the absorbance of malachite green with time at λ=617nm in the presence of different concentrations of ranitidine using the recommended procedure. Ranitidine can be determined from 0.08 to 2.40 g ml-1 with a linear calibration graph and detection limit of 0.026 g ml-1 . The method was successfully applied for the determination of ranitidine in pure ranitidine samples and in ranitidine tablets. The recovery of the analyzed samples were 97-100% with relative standard deviation, sr (%) =1.14 x 10-4 indicating high accuracy and precision of the suggested method. The interference of various cations and anions in the determination of ranitidine was studied

scholarly journals Quality of Ceftriaxone Sodium in Lyophilized Powder for Injection Evaluated by Clean, Fast, and Efficient Spectrophotometric Method

2017 ◽  
Vol 2017 ◽  
pp. 1-4 ◽  
Author(s):  
Patrícia Vidal de Aléssio ◽  
Ana Carolina Kogawa ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Spectrophotometric Method ◽  
Pharmaceutical Formulations ◽  
Uv Detector ◽  
Ceftriaxone Sodium ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference ◽  
Gram Negative Organisms ◽  
Comparison Of The Results

Ceftriaxone sodium, an antimicrobial agent that plays an important role in clinical practice, is successfully used to treat infections caused by most Gram-positive and Gram-negative organisms. Since there are few rapid analytical methods for ceftriaxone analysis to use in the pharmaceutical routine, the aim of this research was to develop a new method able to quantify this cephalosporin. Therefore, a sensitive, rapid, simple UV spectrophotometric method for the determination and quantification of ceftriaxone sodium was proposed. The UV detector was set at 241 nm. Beer’s law obeyed the concentration range of 10–20 µg mL−1. Statistical comparison of the results with a well-established reported method showed excellent agreement and proved that there is no significant difference in the accuracy and precision. Intra- and interday variability for the method were less than 2% relative standard deviation. The proposed method was applied to the determination of the examined drugs in pharmaceutical formulations and the results demonstrated that the method is equally accurate, precise, and reproducible as the official methods.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

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