Separation-free spectrophotometric platforms for rapid assessment of combined antiplatelet therapy in complex matrices

Bioanalysis ◽  
2020 ◽  
Vol 12 (5) ◽  
pp. 335-348 ◽  
Author(s):  
Ahmed Elsonbaty ◽  
Maya S Eissa ◽  
Wafaa S Hassan ◽  
Sara Abdulwahab
Keyword(s):  
Rapid Assessment ◽  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Dual Wavelength ◽  
Therapeutic Drug ◽  
Reference Ranges ◽  
Complex Matrices ◽  
Reliable Determination ◽  
Ich Guidelines ◽  
Mean Centering

Aim: To develop simple and rapid UV-spectrophotometric platforms for the simultaneous quantification of a binary mixture containing clopidogrel bisulphate (CPS) and aspirin (ASP) in complex matrices without prior separation. Experimental: Five mathematical models namely ratio-difference method, mean centering of the ratio spectra, dual wavelength, induced dual wavelength and H-Point Standard Addition method, were utilized for resolving spectral overlap by mathematical processing of ratio and zero-order absorption spectra. Analytes were extracted from tested matrices (whole blood, pharmaceutical formulations and dissolution media buffer) and quantified using the proposed methods. The methods were validated according to ICH guidelines. Results: The developed methods demonstrated limits of detection ranging from 0.67 to 1.09 μg/ml-1 for CPS and 0.49 to 0.71 μg.ml-1 for ASP. All proposed methods allowed for reliable determination of CPS and ASP in complex matrices within reported reference ranges, indicating their potential application for therapeutic drug monitoring and quality control testing.

scholarly journals Three Spectrophotometric Methods for Quantitative Analysis of Duloxetine in Presence of its Toxic Impurity: 1-Naphthol

2020 ◽  
Vol 103 (4) ◽  
pp. 972-979 ◽  
Author(s):  
Ibrahim A Naguib ◽  
Nessreen S Abdelhamid ◽  
Basma H Anwar ◽  
Maimana A Magdy
Keyword(s):  
Pharmaceutical Formulations ◽  
Control Analysis ◽  
Aquatic Life ◽  
Spectrophotometric Methods ◽  
Duloxetine Hydrochloride ◽  
Ich Guidelines ◽  
Mean Centering ◽  
Absorbance Difference ◽  
The Mean

Abstract Background Duloxetine hydrochloride (DUL) is a drug used to treat depression and anxiety. 1-Naphthol is a potential toxic impurity of DUL, as it causes hepatotoxicity in humans, and it is harmful to aquatic life. Objective Three simple, selective, rapid, accurate and precise methods were developed and validated according to International Conference on Harmonization (ICH) guidelines with respect to linearity, accuracy, precision and selectivity for analysis of duloxetine hydrochloride (DUL) in the presence of its potential toxic impurity 1-Naphthol in different laboratory-prepared mixtures and pharmaceutical formulations. Methods Method (A) is the first derivative of the ratio spectra spectrophotometric (1DD) method which allows determination of DUL at 251 nm and 1-Naphthol at 305.2 nm without interference from each other. Method B (dual wavelength) means that two different wavelengths were chosen to each drug, where the absorbance difference at these two wavelengths is equal to zero to the second drug. The chosen two wavelengths for DUL were 221.4 nm and 235.6, where the absorbance difference for 1-naphthol at these two wavelengths was equal to zero. While the chosen wavelengths for 1-naphthol were 247.8 nm and 297 nm, where the absorbance difference for DUL at these two wavelengths was equal to zero. Method (C) is the mean centering of ratio spectra spectrophotometric (MCR) method, which depends on measuring the mean centered values of ratio spectra of both DUL and 1-Naphthol at 226 nm. Results These methods were validated and agreed with the requirements of ICH guidelines with respect to linearity, accuracy, precision and selectivity. Conclusions The results indicate the ability of developed methods to be used for routine quality control analysis of DUL in bulk and pharmaceutical formulations in the presence of its potential impurity 1-Naphthol.

scholarly journals Development and Validation of UV-Spectrophotometric Method for Estimation of Metformin Hydrochloride and Pioglitazone in Tablet Dosage Form

2019 ◽  
Vol 9 (4-A) ◽  
pp. 381-384
Author(s):  
Rupali S. Joshi ◽  
Ajit K. Nangare ◽  
Deepali S. Sanap ◽  
Surekha M. Sase
Keyword(s):  
Dosage Form ◽  
Estimation Method ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Dual Wavelength ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Simple, sensitive, rapid and accurate UV spectroscopic methods have been developed for the estimation of metformin hydrochloride and pioglitazone in tablet dosage forms. Simultaneous estimation and dual-wavelength methods were developed and validated using solvent methanol. Both drugs show linearity at 5-40 µg/ml for both methods. The suggested techniques have been effectively implemented in pharmaceutical formulations to the evaluation of quoted drugs. Recovery research was conducted to verify the method's accuracy, precision. The techniques have been validated under ICH guidelines. Keywords: Metformin hydrochloride, Pioglitazone, Simultaneous estimation method and Dual wavelength method.

Eco-friendly spectrophotometric methods for assessment of alfuzosin and solifenacin in their new pharmaceutical formulation; Green profile evaluation via eco-scale and GAPI tools

2020 ◽  
Vol 16 ◽  
Author(s):  
Mamdouh R. Rezk ◽  
Mina Wadie ◽  
Soheir A. Weshahy ◽  
Mahmoud A. Tantawy
Keyword(s):  
Minor Component ◽  
Time Saving ◽  
Prostate Hyperplasia ◽  
Spectrophotometric Methods ◽  
Ratio Difference ◽  
Ich Guidelines ◽  
Mean Centering ◽  
Benign Prostate ◽  
Urological Diseases

Background: Alfuzosin is recently co-formulated with solifenacin for relieving two coincident urological diseases, namely; benign prostate hyperplasia and overactive bladder Objective: Herein, green, simple and rapid spectrophotometric methods were firstly developed for simultaneous determination of the two cited drugs in their co-formulated pharmaceutical capsule Methods: Alfuzosin, which is the major component in the dosage form, was directly assayed at its extended wavelength at 330.0 nm. The challenging spectrum of the minor component, solifenacin, was resolved by five spectrophotometric methods, namely; dual wavelength (DW) at 210.0 & 230.0 nm, first derivative (1D) at 222.0 nm, ratio difference (RD) at 217.0 - 271.0 nm , derivative ratio (1DD) at 223.0 and mean centering of ratio spectra (MC) at 217.0 nm Results: The Proposed methods were successfully validated as per ICH guidelines. Alfuzosin showed linearity over the range of 4.0 - 70.0 μg/mL, while that of solifenacin were 4.0 - 50.0 μg/mL for DW, 2.0 - 70.0 μg/mL for 1D and RD methods, 1.0 - 70.0 μg/mL for 1DD and 4.0 - 70.0 μg/mL for MC method. Statistical comparison with their official ones showed no noticeable differences. The methods showed good applicability for assaying drugs in their newly combination. Besides eco-scale, the greenness profile of the methods was assessed and compared with the reported spectrophotometric one via the newest metric tool; green analytical procedure index (GAPI). Conclusions: The proposed methods are superior in not only being smart, accurate, selective, robust and time-saving, but also in using distilled water as an eco-friendly and cheap solvent

RP-HPLC METHOD DEVELOPMENT FOR THE ASSAY OF AMPHOTERICIN B

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (02) ◽  
pp. 16-20
Author(s):  
L Mohankrishna ◽  
◽  
P. J. Reddy ◽  
B. P Reddy. ◽  
P. Navya
Keyword(s):  
Amphotericin B ◽  
Mobile Phase ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Phase Combination ◽  
Hplc Method Development

A sensitive and precise HPLC procedure has been developed for the assay of amphotericin B in bulk samples and pharmaceutical formulations by using a C18 column [Kromosil, C18, (5 µm, 4.6mm x 250 mm; Make. Waters)], and mobile phase combination is 1% formic acid in water and acetonitrile in ratio of 45:55 V/V. The procedure has been validated as per the ICH guidelines. The λmax of detection was fixed at 407 nm, so that there was less interference from mobile phase with highest sensitivity according to UV analysis. Calibration plots were linear in the range of 10-100 µg/mL and the LOD and LOQ were 0.02 µg/mL and 0.06 µg/mL respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of amphotericin B in different formulations.

Therapeutic Drug Monitoring of Lamotrigine, Lacosamide, and Levetiracetam in Dried Capillary Blood – Determination of Conversion Factors for Serum-Based Reference Ranges

2021 ◽  
Vol Publish Ahead of Print ◽  
Author(s):  
Dennis Klimpel ◽  
Anne Hagemann ◽  
Christian G. Bien ◽  
Bertin Dufaux ◽  
Theodor W. May ◽  
...  
Keyword(s):  
Therapeutic Drug Monitoring ◽  
Drug Monitoring ◽  
Capillary Blood ◽  
Therapeutic Drug ◽  
Reference Ranges ◽  
Conversion Factors

Validated HPTLC Method for the Estimation of Oxetacaine in Pharmaceutical Formulations

2021 ◽  
pp. 5668-5672
Author(s):  
Kavitha J ◽  
Bonda Vismitha ◽  
Kokilambigai KS ◽  
Seetharaman R ◽  
Lakshmi KS
Keyword(s):  
Mobile Phase ◽  
Glacial Acetic Acid ◽  
Current Method ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Relieve Pain ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Chromatographic Resolution ◽  
Hptlc Method

Oxetacaine is a potent local anesthetics used to relieve pain associated with peptic ulcer. The current method details about a rapid, accurate and precise HPTLC technique for the assessment of Oxetacaine in Pharmaceutical formulation. Chromatographic resolution was carried out on precoated HPTLC plates (Silica gel 60 F254 on Aluminum plate) employing methanol: water: glacial acetic acid (8: 1.8: 0.2 v/v/v) as mobile phase. Densitometric assessment was carried out at 220nm [Camag TLC Scanner III with winCATs software (version – 1.3.4)]. The drug was identified with a Rf value of 0.61. The reliability of the projected method was ascertained by evaluating various validation parameters as per ICH guidelines. The proposed technique can evaluate ten or more formulation units concurrently in a single run and affords a more rapid and cost-effective QC tool for regular analysis of Oxetacaine in pharmaceutical formulations.

Reversible cognitive impairment associated with a high free fraction but subtherapeutic total blood level of valproic acid due to hypoalbuminemia in a bipolar patient

2017 ◽  
Vol 41 (S1) ◽  
pp. S420-S420
Author(s):  
G. Dautzenberg ◽  
M. Nederlof ◽  
E. Heerdink ◽  
A. Beekman
Keyword(s):  
Valproic Acid ◽  
Cognitive Impairment ◽  
Binding Capacity ◽  
Free Fraction ◽  
Bipolar Patient ◽  
Therapeutic Drug ◽  
Blood Levels ◽  
Reference Ranges ◽  
Total Blood ◽  
Pharmacologically Active

Valproic acid (VPA) is widely used in the treatment of epilepsy and bipolar disorder. It is largely bound to serum proteins (80–95%) in particular albumin, with a saturable binding capacity. Under conditions of hypoalbuminemia, protein binding of VPA will decrease and its pharmacologically-active free fraction will rise, even to toxic levels while measuring subtherapeutic VPA total blood levels [1].We present an elderly bipolar patient with (sub)clinical total levels of VPA and a high free fraction of VPA due to hypoalbuminemia (14–24 g/L) leading to severe reversible cognitive impairment.VPA and the free fraction in particular, was the most likely cause of the cognitive impairment [2]. There was a time-correlation with increasing blood levels of total VPA (68 mg/L, reference 80–120 mg/L [3]), notably the free fraction (37.5 mg/L, reference 5–15 mg/L), and the intoxication.For therapeutic drug monitoring in laboratories, generally, total VPA concentrations (free + protein-bound) are measured instead of free fractions, due to technical difficulties, a lack of established reference ranges [4] and (inter)national guidelines [5,6] not requiring it. This presentation and literature points out that it is clinically relevant to measure the free fraction [7,8], especially in patients with hypoalbuminemia [9–11] to prevent unnecessary side effects and toxicity.We recommend measuring albumin during VPA use; particularly in patients with nephrotic syndrome, liver disease [12] or older adults [13–15]. Hypoalbuminemia demands a free fraction measurement.Disclosure of interestThe authors have not supplied their declaration of competing interest.

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.

QBD BASED RP-HPLC METHOD FOR SCREENING AND ANALYSIS OF TELAPRAVIR AND 7 OTHER ANTIRETROVIRAL AGENTS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 20-33
Author(s):  
N. S Kumar ◽  
◽  
R Kumaraswamy ◽  
S. Shantikumar ◽  
D. Paul
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Full Factorial

The present study describes the separation and simultaneous estimation of eight anti-retroviral drugs, namely, Telaprevir (TPV), Emtricitabine (ECB), Fosamprenavir (FANV), Tenofavir (TNF), Ritonavir (RNV), Raltegravir (RGV) and Oseltamivir (OSMV) and Zidovudine (ZDV) as an active pharmaceutical ingredient, by RP-HPLC method by applying the principles of Quality by Design (QbD). An application of DoE (Design of Experiments) full factorial design was used for initial screening and optimization. The final optimized method consists of separation being carried out on a Fortis C18 column (150 mm × 4.6 mm, 5μ particle size) using acetonitrile and 10 mm ammonium formate buffer (pH 3 adjusted with formic acid) using a gradient program. The quantitative evaluation was performed with a diode array detector at 251 nm and 230 nm with a flow rate of 1 mL min–1. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the International Conference on Harmonization (ICH) guidelines. The method is selective, precise, robust and accurate and can be used for routine analysis of pharmaceutical formulations in quality control and counterfeit screening.

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