Spectrophotometric Determination of Zolmitriptan in Pure Form and in Tablets Through Charge Transfer Complex Reaction

2019 ◽  
Author(s):  
Safwan Ashour
Keyword(s):  
Charge Transfer ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Dominant Mode ◽  
Pure Form ◽  
Apert Syndrome ◽  
Charge Transfer Complexes ◽  
Midfacial Hypoplasia ◽  
Limit Of Quantitation

Apert syndrome (AS) a type of acrocephalosyndactyly is a rare congenital disorder with autosomal dominant mode of transmission that consists of craniofacial synostosis, midfacial hypoplasia and bilateral limb syndactyly. Patients present in early childhood for multiple surgeries which make it imperative to know about various anaesthetic implications like difficult airway ventilation, airway hyper reactivity, associated congenital anomalies, increased airway secretions and deranged temperature thermoregulation associated with this syndrome. The patient should be thoroughly evaluated preoperatively and managed accordingly. We discuss the successful management of a three and a half years old male child two simple, rapid and selective colorimetric methods were developed for the determination of zolmitriptan (ZMT) in pure form and pharmaceutical preparations. These methods are based on the directly formation of charge-transfer complexes between ZMT and m-nitrophenol (MNP) in aqueous medium (ZMT: MNP, 1:1) and 2,4-dinitrophenol (DNP) in ethanol:water (80:20). The developed method involves formation of coloured complexes (1:1) of ZMT with MNP and DNP. The yellow formed complexes were quantitatively measured at 400 and 440 nm for ZMT-MNP and ZMT-DNP, respectively. Beer's law was obeyed in the concentration ranges of 3.0–260 μg/mL for MNP and 3.5–120 μg/mL for DNP. Limit of detection and limit of quantitation for MNP were calculated as 0.58 and 1.75 μg/mL, respectively, and for DNP were 0.32 and 0.97 μg/mL, respectively. The method was validated with respect to accuracy, robustness and selectivity. The proposed method has been successfully applied for the determination of ZMT in tablets.

scholarly journals Determination of Atenolol and Trimetazidine in Pharmaceutical Tablets and Human Urine Using a High Performance Liquid Chromatography-Photo Diode Array Detection Method

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Walaa El-Alfy ◽  
Omnia A. Ismaiel ◽  
Magda Y. El-Mammli ◽  
Abdalla Shalaby
Keyword(s):  
Human Urine ◽  
Limit Of Detection ◽  
Pure Form ◽  
Urine Samples ◽  
Dihydrogen Phosphate ◽  
Simple Liquid ◽  
Pharmaceutical Tablets ◽  
Limit Of Quantitation ◽  
Precision And Accuracy

A simple RP-HPLC-PDA method for determination of atenolol (ATN) and trimetazidine (TMZ) in human urine and tablets has been developed. Analytes were separated on a Caltrex BI column (125× 4.0 mm, 5 μm) with 25mM potassium dihydrogen phosphate pH 3.3, methanol, and acetonitrile mobile phases. The PDA detector was operated at 210 nm for TMZ and 225 nm for ATN and the flow rate was 1.0 mL/ min. Linearity was obtained over a concentration range of (1.0-100 μg/mL) for both analytes in standard solutions and the method was successfully applied for determination of target analytes in their pharmaceutical tablets. Excellent linearity was also obtained over concentration ranges of (0.25-25 μg/mL) and (0.5-25 μg/mL) in human urine for TMZ and ATN, respectively. A simple liquid-liquid extraction was applied for urine sample clean-up and a gradient method was used for chromatographic separation. The lower limit of quantitation (LOQ) was 0.99 and 0.60 μg/mL for ATN and TMZ, respectively. The limit of detection (LOD) was 0.30 and 0.18 μg/mL for ATN and TMZ, respectively. Inter- and intraday precision and accuracy for ATN were within ±1.89% in pure form and within ±2.85% in urine samples. Inter- and intraday precision and accuracy for TMZ were within ± 3.99% in pure form and within ± 3.19% in urine samples.

Micellar-Enhanced Spectrofluorimetric Method for Quantification of Diclofenac Potassium in Pure Form, in Pharmaceutical Preparations and Human Plasma

2021 ◽  
Vol 58 (6) ◽  
pp. 427-434
Author(s):  
Muhammad Naeem Khan ◽  
Irum ◽  
Saba Gul ◽  
Muslima ◽  
Muhammad Mursaleen
Keyword(s):  
Human Plasma ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Pure Form ◽  
Fluorescence Signal ◽  
Spectrofluorimetric Method ◽  
Relative Standard

Abstract A rapid, simple and economical spectrofluorimetric method for the determination of diclofenac potassium in pure form, in pharmaceutical preparations and in human plasma has been developed. The method is based on the enhancement of the fluorescence signal of diclofenac potassium by the addition of sodium dodecyl sulphate in McIvaine buffer with a pH of 5. Different experimental conditions such as buffer type, pH, type and concentration of surfactants were investigated. The fluorescence intensity of the solution was recorded at 361 nm after excitation at 243 nm. The method shows linearity in the concentration range of 0.2 μg mL–1–10 μg mL–1 with a good correlation coefficient of 0.997. The relative standard deviation value was 3.62 (n = 7). The limit of detection and limit of quantification were calculated to be 2.84 × 10–3 μg mL–1 and 9.47 × 10–3 μg mL-1, respectively. The effect of excipients and co-administrated drugs was investigated and no interference was observed. The method was successfully applied for the determination of diclofenac potassium in pure form, in pharmaceutical products and in human plasma. The percentage recoveries obtained ranged from 100.25% to 102.16% for pure form and 97.50% to 102.00% for pharmaceutical products and from 98.50% to 101.67% for human plasma.

scholarly journals Development and Validation of New RP-HPLC Method for Simultaneous Determination of Methyl and Propyl Parabens with Levetiracetam in Pure Form and Pharmaceutical Formulation

2016 ◽  
Vol 2016 ◽  
pp. 1-5 ◽  
Author(s):  
Soad S. Abd El-Hay ◽  
Mostafa S. Mohram
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Limit Of Quantitation

A simple and robust high-performance liquid chromatography (HPLC) method is described for the assay for levetiracetam (LTC), methyl paraben (MHB), and propyl paraben (PHB) either in their pure form or in commercial Levepsy® syrup. The method is selective and stability indicating and all chromatographic conditions were studied to obtain adequate separation of LTC, MHB, and PHB from their degradation products and from excipients. The HPLC separation was carried out on a RP C18 Hypersil BDS analytical column (150 mm × 4.6 mm ID) using gradient elution system. The mobile phase flow rate was 1.5 mLmin−1 and the column temperature was kept at 40°C. Complete separation of the studied components was obtained within a cycle time of 8 min. LTC, MHB, and PHB were eluted at 1.56, 5.86, and 7.85 min, respectively. Detection was carried out at 240 nm using a dual wavelength detector. The method has been validated for linearity, accuracy, precision, specificity, limit of detection, limit of quantitation, robustness, and ruggedness. The proposed method was successfully applied for the determination of LTC in the presence of parabens in Levepsy syrup.

scholarly journals CHARGE-TRANSFER COMPLEXES OF CHLORPHENOXAMINE HYDROCHLORIDE WITH CHLORANILIC ACID, 2,3-DICHLORO-5,6-DICYANO-1,4-BENZOQUINONE AND 7,7,8,8-TETRACYANOQUINODIMETHANE AS π-ACCEPTORS

2019 ◽  
pp. 117-123
Author(s):  
AKRAM M. EL-DIDAMONY ◽  
MOUNIR Z. SAAD ◽  
GEHAD M. RAMADAN
Keyword(s):  
Charge Transfer ◽  
Limit Of Detection ◽  
Standard Free Energy ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Charge Transfer Complexes ◽  
Reaction Products ◽  
Chloranilic Acid ◽  
Accuracy And Precision ◽  
Ct Complex

Objective: To develop simplified, accurate and precise visible spectrophotometric strategies for the assay of chlorphenoxamine hydrochloride (CPX) in pure drug and in its pharmaceutical preparations. Methods: The described methods depended on the formation of charge-transfer (CT) complexes of intense color between CPX as donor with three π-acceptors, chloranilic acid (CLA), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), and 7,7,8,8-tetracyanoquinodimethane (TCNQ) and the colored reaction products were estimated spectrophotometrically at 520 nm, 460 nm and 840 nm for CLA, DDQ, and TCNQ complexes, individually. All the optimum conditions were established. The proposed methods were validated in term of linearity, limit of detection as per the international conference on harmonization guidelines ICH Q2 (R1). Results: The complexes obeyed Beer’s law in the concentration range of 16-144, 6-54 and 4-76 μg/mlwith molar absorptivity at 0.30×104, 0.68×104 and 0.58×104 l/mol/cm for CLA, DDQ, and TCNQ, individually. According to Benesi-Hildebrand plots, the association constants and changes of standard free energy were determined. 1:1 was the ratio of composition of the formed CT-complex. Conclusion: The obtained results revealed that the developed method can be applied successfully for the determination of CPX in drug formulations samples with good accuracy and precision.

Development and Validation of Novel UPLC-MS/MS Method for the Analysis of Macitentan in Pharmaceutical Formulations

2019 ◽  
Vol 15 (5) ◽  
pp. 554-559
Author(s):  
Mevlut Albayrak ◽  
Alptug Atila
Keyword(s):  
Atmospheric Pressure Chemical Ionization ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Ultra Performance Liquid Chromatography ◽  
Pure Form ◽  
Column Temperature ◽  
Limit Of Quantitation

Introduction: Macitentan is an endothelin receptor antagonist drug used in the treatment of pulmonary arterial hypertension. Materials and Methods: A new, sensitive, simple, accurate and rapid ultra-performance liquid chromatography in combination with tandem triple quadruple mass spectrometry (UPLC-MS/MS) method has been developed and validated for the determination of macitentan in pharmaceutical formulations. Macitentan and bosentan which are used as internal standard (IS) were detected using atmospheric pressure chemical ionization (APCI) in positive ion, multiple reaction monitoring (MRM) mode by monitoring mass transitions (precursor to product) m/z 589.1→203.3 and 552.6→311.5, respectively. Chromatographic separation was carried out on reverse phase C18 column (5 µm, 4.6 * 150 mm). Water containing 0.2 % acetic acid in acetonitrile (10:90, v/v) was used as the mobile phase in the isocratic elution. The system was optimized with injection volume of 10 µL, column temperature of 35 °C and flow rate of 1 mL min-1 Retention times were 1.97 min for macitentan and 1.72 min for IS. Results and Discussion: The calibration curve with a high correlation coefficient (0.9997) was linear range 0.5-500 ng mL-1. The lower limit of quantitation (LLOQ) and average recovery values were determined as 0.5 ng mL-1 and 99.7 %, respectively. The developed novel method has been successfully applied for the determination of macitentan in pure form and pharmaceutical formulations. Conclusion: The present method is the first study developed and validated for the determination of macitentan from the pharmaceutical preparations and pure form by UPLC-MS/MS method in the literature.

scholarly journals Use of the Charge Transfer Reactions for the Spectrophotometric Determination of Risperidone in Pure and in Dosage Forms

2013 ◽  
Vol 2013 ◽  
pp. 1-6
Author(s):  
Hemavathi Nagaraju Deepakumari ◽  
Hosakere Doddarevanna Revanasiddappa
Keyword(s):  
Charge Transfer ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Charge Transfer Complexes ◽  
Chloranilic Acid ◽  
Colored Complex ◽  
Relative Standard ◽  
Complexation Reactions

The aim of study was to develop and validate two simple, sensitive, and extraction-free spectrophotometric methods for the estimation of risperidone in both pure and pharmaceutical preparations. They are based on the charge transfer complexation reactions between risperidone (RSP) as n-electron donor and p-chloranilic acid (p-CA) in method A and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in method B as π-acceptors. In method A, RSP reacts with p-CA in methanol to produce a bright pink-colored chromogen measured at 530 nm whereas, in method B, RSP reacts with DDQ in dichloromethane to form orange-colored complex with a maximum absorption at 460 nm. Beer's law was obeyed in the concentration range of 0–25 and 0–50 μg/mL with molar absorptivity of and L/moL/cm for RSP in methods A and B, respectively. The effects of variables such as reagents, time, and stability of the charge transfer complexes were investigated to optimize the procedures. The proposed methods have been successfully applied to the determination of RSP in pharmaceutical formulations. Results indicate that the methods are accurate, precise, and reproducible (relative standard deviation %).

scholarly journals Spectrophotometric determination of Valsartan in pure form and in its pharmaceutical preparations

2021 ◽  
Vol 26 (4) ◽  
Author(s):  
Qabas Rashid ◽  
Ruwaida Farman Salih
Keyword(s):  
Correlation Coefficient ◽  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Pure Form ◽  
Chromogenic Reagent

An easy, rapid and economical spectrophotometric method for  determination of  Valsartan (Val), by reaction with 4-chloro-7-nitrobenzofurazan (NBD-Cl) as reagent in an alkaline interemediate. This method is based on the forming of product between (Val) and the chromogenic reagent (NBD-Cl), to produce a brown color at (pH 11.9) and λmax. 470 nm.  Beer’s Law is obeyed at the concentrations range of (0.4-14.8 µg/ml), with molar absorptivity of (1.05×104 L/mol.cm) and correlation coefficient 0.9827, The limit of detection was 0.557 µg/ml. The suggested method was prosperity implement to the determination of (Val) in  pure form and in its pharmaceutical formulations (tablets).

scholarly journals Development and Validation of Spectrophotometric Methods for the Determination of Rasagiline in Pharmaceutical Preparations

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Serife Evrim Kepekci Tekkeli ◽  
Armağan Önal ◽  
Fatemeh Bahadori
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Dosage Forms ◽  
Chloranilic Acid ◽  
Spectrophotometric Methods ◽  
H Nmr ◽  
Limit Of Quantitation ◽  
Development And Validation

This study presents three simple, rapid, and accurate spectrophotometric methods for the determination of Rasagiline (RSG) in pharmaceutical preparations. The determination procedures depend on the reaction of RSG with chloranilic acid for method A, tetrachloro-1,4-benzoquinone for method B, and 7,7,8,8-tetracyanoquinodimethane for method C. The colored products were quantitated spectrophotometrically at 524, 535, and 843 nm for methods A, B, and C, respectively. Different variables affecting the reaction were optimized. Linearity ranges of the methods with good correlation coefficients (0.9988–0.9996) were observed as 25–300 µg mL−1, 25–350 µg mL−1, and 50–500 µg mL−1for methods A, B, and C, respectively. The formation of products takes place through different mechanisms. The sites of interaction were confirmed by elemental analysis using IR and1H-NMR spectroscopy. The validation of the methods was carried out in terms of specificity, linearity, accuracy, precision, robustness, limit of detection, and limit of quantitation. No interference was observed from concomitants usually present in dosage forms. The methods were applied successfully to the determination of RSG in pharmaceutical preparations.

Establishment and Validation of a Sensitive Method for the Detection of Pregabalin in Pharmacological Formulation by GC/MS Spectrometry

2019 ◽  
Vol 15 (2) ◽  
pp. 165-171 ◽  
Author(s):  
Wael Abu Dayyih ◽  
Mohammed Hamad ◽  
Eyad Mallah ◽  
Alice Abu Dayyih ◽  
Kenza Mansoor ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Pharmacological Preparation ◽  
Gas Chromatography Mass Spectroscopy ◽  
Anticonvulsant Activities

Background: A gas chromatography and mass spectrometry (GC/MS) procedure was developed and validated for the evaluation and quantification of pregabalin (PGN) in pharmaceutical preparations. </P><P> Introduction: Pregabalin is a γ-amino-n-butyric acid derivative used as an antiepileptic drug for the management of fibromyalgia, and has analgesic, anxiolytic, and anticonvulsant activities. Few studies have been reported on the determination of PGN content in pharmaceutical preparations involving gas chromatography - mass spectroscopy. Methods: Pregabalin was extracted with MSTFA/NH4F/β- mercapto-ethanol at 60°C for 30 min. The acquired derived molecule of pregabalin was identified by specific ion monitoring mode applying the analytical ions m/z 232 and 331. Propranolol was used as Internal Standard (IS). The following validation parameters were taken into consideration: precision, linearity, accuracy, stability, specificity, robustness, ruggedness, Limit Of Detection (LOD) and Limit Of Quantitation (LOQ). Results: The method was selective, precise, sensitive, linear and specific. The linearity of the method was between 3.5 and 300 ng/ml. The precise values were ≤ 3.62% of both intra- and interday validation. The LOD accurate values for Intraday and interday validation were in the range of -0. 25 -2.05%. While LOQ accurate values for intraday and interday were 1.5x10-6 and 3.5 x10-6mg/ml, respectively. Conclusion: Therefore, the developed GC-MS method was effectively implemented to identify PGN in a pharmacological preparation.

Extractive Spectrophotometric Methods for Determination of Chlorpheniramine Maleate in Pure Form, Pharmaceutical Preparations and Biological Fluids

2017 ◽  
Vol 75 ◽  
pp. 11-24
Author(s):  
Marwa El Badry Mohamed ◽  
Eman Y.Z. Frag ◽  
Hana A. El-Boraey ◽  
Safa S. El-Sanafery
Keyword(s):  
Blood Serum ◽  
Limit Of Detection ◽  
Biological Fluids ◽  
Ion Pairs ◽  
Pharmaceutical Preparations ◽  
Pure Form ◽  
Stoichiometric Ratio ◽  
Bromocresol Purple ◽  
Chlorpheniramine Maleate

In this study a simple, rapid and sensitive spectrophotometric method was developed for the determination of an antihistaminic drug chlorpheniramine maleate (CPM) in pure form, pharmaceutical preparations, spiked humane urine and spiked blood serum. This method was based on the formation of ion-pairs between the basic nitrogen of the CPM drug and four chromogenic reagents namely bromocresol purple (BCP), alizarine Red S (ARS), eriochrome cyanine R (ECR), and cresol red (CR). The extracted colored ion-pairs were measured spectrophotometrically at 390, 425, 503 and 408 nm for BCP, ARS, ECR and CR reagents, respectively. The different parameters that affect the color development between CPM drug and dyestuff reagents were extensively studied to determine the optimal conditions for the assay procedure. The reaction was studied as a function of the volume of reagents, nature of solvent, temperature, reaction time and stoichiometric ratio between the CPM drug and the reagents. Beer’s law was valid over the concentration ranges of 1-30, 1-10, 2-120 and 4-120 μg mL-1 of CPM drug using BCP, ARS, ECR and CR reagents, respectively. The Sandell sensitivity, molar absorptivity, limit of detection and limit of quantification were determined. Applications of the proposed procedure to the analysis of the pharmaceutical preparations, spiked humane urine and spiked blood serum gave reproducible and accurate results without any interference from excipients. The results obtained by the proposed method were in good agreement with those obtained by reported method. The method can be suggested for the routine analysis of the cited drug.

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