scholarly journals Optimization and validation of a new chromatographic method for the assay of veterinary formulation

2019 ◽  
Vol 10 (3) ◽  
pp. 218-223
Author(s):  
Hany Hunter Monir ◽  
Adel Magdy Michael ◽  
Christine Kamal Nessim ◽  
Yasmin Mohamed Fayez ◽  
Nahla Salah Elshater
Keyword(s):  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Fixed Dose ◽  
Selective Determination ◽  
Ich Guidelines ◽  
Significant Difference ◽  
Dose Combination ◽  
Student’S T

New, validated and accurate reversed phase HPLC method with UV detection has been established for simultaneous determination of a veterinary binary mixture of doxycycline hydrochloride (DOX) and tylosin tartrate (TYT). The stationary phase was ACE- 126-2546 AQ C-18 (250 × 4.6 mm i.d., 5 μm particle size) column at 25 °C, in an isocratic mode, using mobile phase containing a mixture of methanol: acetonitrile: distilled water in the ratio of 60:20:20 (v:v:v), with 0.01% trichloroacetic acid at the flow rate of 0.8 mL/min and UV detection was performed at 270 nm. The retention times were 4.02±0.01 and 5.62±0.01 mins for DOX and TYT, respectively. Selective determination of the cited veterinary drugs has been developed in their formulation. The method was found to be linear over 1-50 µg/mL for DOX and TYT with mean percentage recoveries 99.62±1.220 and 100.09±1.104%. The method was proven to be accurate, precise and specific. The obtained results were statistically compared with those of the official and reported methods; using Student’s t test, F test and one-way ANOVA, showing no significant difference with high accuracy. Specificity of the applied method was assessed by analysing the laboratory-prepared mixtures and their combined dosage form. The developed method was confirmed according to ICH guidelines. The validated method can be considered as alternative and basic method for the routine determination of this fixed dose combination with minimum sample preparation.

Selective Determination of Entecavir in the Presence of Its Oxidative Degradate by Spectrophotometric and Chromatographic Methods

2021 ◽  
Author(s):  
Heba M El-Sayed ◽  
Laila E Abdel Fattah ◽  
Hisham E Abdellatef ◽  
Maha A Hegazy ◽  
Mai M Abd El-Aziz
Keyword(s):  
High Selectivity ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Peak Amplitude ◽  
Quality Analysis ◽  
Official Method ◽  
Selective Determination ◽  
Significant Difference ◽  
Development And Validation

Abstract Background Entecavir (ENT) is an antiretroviral agent prescribed for treatment of HBV and HIV. Objective Development and validation of three simple, sensitive, selective, and precise methods for determination of ENT in presence of its oxidative degradation product (ENT deg.). Methods The first method was based on second derivative (D2) spectrophotometry through measuring the peak amplitude of D2 spectra at 293.6 nm. The second one is mean centering of the ratio spectra (MCR), which allowed measuring the peak amplitude at 280.0 nm. While the third method was HPLC; where ENT was separated from ENT deg. using Zobrax C18column and methanol: water (30:70, v/v), pH 3 as a mobile phase. The three developed methods were validated according to ICH guidelines. Results Linearity range of ENT was 5.00–50.00 μg/mL for both D2and MCR. However, higher sensitivity was achieved using HPLC (1.00–50.00 μg/mL). Accuracy of ENT were 100.60%±0.547, 101.55%±1.2071 and 100.61%±1.207 for D2, MCR and HPLC methods, respectively, and precision was within 1.280. Conclusions The developed methods were successfully applied for the determination of ENT in Tecavir® tablets without interference from ENT deg. They showed no significant difference compared with the official method as well as they could be applied in the quality analysis of ENT with high selectivity, accuracy, and precision. Highlights ENT was quantified using two spectrophotometric (D2 and MCR) methods and an HPLC method in presence of ENT deg. The proposed methods were applied to analysis of ENT tablets with high selectivity, sensitivity, and accuracy.

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

Molecular and Quantum Mechanical Study for the Separation of Cefprozil in the Presence of Its Alkaline Degradation Product Using RP-HPLC with UV Detection

2017 ◽  
Vol 100 (2) ◽  
pp. 392-399 ◽  
Author(s):  
Khalid A M Attia ◽  
Mohammed W I Nassar ◽  
Mohamed B El-Zeiny ◽  
Ahmed Serag
Keyword(s):  
Degradation Product ◽  
Generation Cephalosporin ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Quantum Mechanical ◽  
Rp Hplc ◽  
Quantum Mechanical Study ◽  
Alkaline Conditions

Abstract A reversed-phase HPLC method (RP-HPLC) with UV detection was developed and validated for the quantitative determination of cefprozil, a second-generation cephalosporin. Due to β-lactam ring instability under alkaline conditions, this RP-HPLC method was applied for the determination of cefprozil in the presence of its possible degradation product. The interactions that govern the separation process with stationary phase were investigated at both molecular and quantum mechanical levels. Moreover, electrostatic potential maps were generated to determine the sites of interaction with mobile phase. The suggested method was validated in compliance with International Conference on Harmonization guidelines and successfully applied for the determination of cefprozil in its commercial pharmaceutical formulation.

scholarly journals Validated Stability Indicating Chromatographic Methods for Quantification of Imidocarb Dipropionate; Application for the Determination of Its Residues in Bovine Meat and Milk Samples

2020 ◽  
Vol 103 (4) ◽  
pp. 980-988
Author(s):  
Ghada AbdElHamid Sedik ◽  
Doha Mohamed Naguib ◽  
Fahima Morsy ◽  
Hala Elsayed Zaazaa
Keyword(s):  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Milk Samples ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Imidocarb Dipropionate ◽  
Tlc Plates

Abstract Background Imidocarb dipropionate (IMD) is an immunomodulator agent commonly used for treatment of anaplasmosis in cattle. Objective Thus, two sensitive, specific, and precise stability-indicating chromatographic methods have been developed, optimized, and validated for its determination in presence of its acid, alkaline, and oxidative stressed degradation products. Method The first method is based on separation of IMD and its forced induced degradation products on reversed phase cyano column using isocratic elution system consisted of sodium acetate buffer–methanol–acetonitrile (55: 30:15, v/v/v), pH 4.6 at a flow rate of 1.2 mL/min, and UV detection at 254 nm. The second method utilized TLC combined with densitometric determination of the separated bands at 254 nm. The separation was achieved using silica gel 60 F254 TLC plates with a mixture of ethyl acetate–methanol–ammonia–water (8.5:1:0.5:0.2, v/v/v/v) as a developing system. Results HPLC analysis was applied in range of 0.25–40 µg/mL with LOD of 0.073 µg/mL. While densitometric measurements showed linearity in the range of 0.1–1.8 µg/band with LOD of 0.02 µg/band. Conclusions The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of IMD in its commercial veterinary formulations with good recoveries. Furthermore, the proposed HPLC method was extended to the determination of IMD residues in bovine meat and milk samples Highlights Bovine meat, HPLC, Imidocarb dipropionate, Milk, TLC.

Ultra-Performance Liquid Chromatographic and Densitometric Methods for Sensitive Determination of Xipamide and Triamterene in Pure and Pharmaceutical Dosage Forms

2021 ◽  
Author(s):  
N V Fares ◽  
Haitham A El Fiky ◽  
Amr M Badawey ◽  
Maha F Abd El Ghany
Keyword(s):  
Acetic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detection ◽  
Pharmaceutical Dosage Forms ◽  
Selective Determination ◽  
Liquid Chromatographic

Abstract Background Validated UPLC method and TLC densitometric method were prescribed for determination of antihypertensive components. Objectives: To establish and validate rapid and accurate Ultra performance liquid chromatographic (UPLC) and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. Methods The first method; UPLC method, depended on using Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm), as the column, mobile phase composed of (acetonitrile-water) (70 + 30, v/v) adjusted by acetic acid to obtain (pH 3), 0.2 mL/min flow rate and UV detection at 231.4 nm. The second method was a thin layer chromatography (TLC) densitometric method, separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase and UV detection at 300.0 nm. Results The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. Conclusions The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), lower detection limit less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL) and lower flow rate other than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). Highlights Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixture of Xipamide and Triamterene with LOD less than 0.076 µg/mL for both drugs.

scholarly journals A rapid stability-indicating, fused-core HPLC method for simultaneous determination of β-artemether and lumefantrine in anti-malarial fixed dose combination products

2013 ◽  
Vol 12 (1) ◽  
pp. 145 ◽  
Author(s):  
Sultan Suleman ◽  
Kirsten Vandercruyssen ◽  
Evelien Wynendaele ◽  
Matthias D’Hondt ◽  
Nathalie Bracke ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Hplc Method ◽  
Fixed Dose Combination ◽  
Fixed Dose ◽  
Stability Indicating ◽  
Dose Combination
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