scholarly journals Development and application of a validated HPLC method for the analysis of dissolution samples of mexiletine hydrochloride capsules

2010 ◽  
Vol 75 (7) ◽  
pp. 975-985 ◽  
Author(s):  
Dragan Milenovic ◽  
Zoran Todorovic
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
In Vitro Dissolution ◽  
Selective Method ◽  
Dissolution Studies ◽  
Detection And Quantification

The aim of this work was to develop and validate a simple, efficient, sensitive and selective method for the analysis of dissolution samples of mexiletine hydrochloride capsules by HPLC without the necessity of any time-consuming extraction, dilution or evaporation steps prior to drug assay. Separation was performed isocratically on a 5 ?m LiChrospher 60, RP-Select B column (250 x 4 mm ID) using the mobile phase buffer-acetonitrile (60:42, v/v) at a flow rate of 1.2 mL min-1 and UV detection at 262 nm. The elution occurred in less than 10 minutes. The assay was linear in the concentration range 50-300 ?g mL-1 (r2 = 0.9998). The validation characteristics included accuracy, precision, linearity, specificity, limits of detection and quantification, stability, and robustness. Validation acceptance criteria were met in all cases (the percent recoveries ranged between 100.01 and 101.68 %, RSD < 0.44 %). The method could be used for the determination of mexiletine hydrochloride and for monitoring its concentration in in vitro dissolution studies.

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 Optimization of RP-HPLC method with UV detection for determination of ursodeoxycholic acid in pharmaceutical formulations

2020 ◽  
Vol 66 (1) ◽  
pp. 85-90
Author(s):  
Zhaklina Poposka Svirkova ◽  
Zorica Arsova-Sarafinovska ◽  
Aleksandra Grozdanova
Keyword(s):  
Ursodeoxycholic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Hplc Method ◽  
Uv Detection ◽  
Rp Hplc ◽  
Ich Guidelines

Due to the low absorptivity of bile acids, the aim of this study was to develop and validate a simple and sensitive HPLC/UV method for quantification of ursodeoxycholic acid (UDCA) in pharmaceutical formulations. Effective separation was achieved on C18 end–capped column, with gradient elution of a mobile phase composed of 0.001 M phosphate buffer (pH 2.8±0.5) – acetonitrile mix, at flow rate 1.5 mL min-1, UV detection at 200 nm and injection volumes were 50 µL. The proposed HPLC method was fully validated according to the ICH guidelines and it was found to be simple, accurate, precise and robust. Key words: ursodeoxycholic acid, HPLC/UV, pharmaceutical formulations, validation

RP-HPLC Method for Simultaneous Determination of Sofosbuvir and Ledipasvir in Tablet Dosage Form and Its Application to In Vitro Dissolution Studies

2016 ◽  
Vol 79 (23-24) ◽  
pp. 1605-1613 ◽  
Author(s):  
Bakht Zaman ◽  
Faisal Siddique ◽  
Waseem Hassan
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Hplc Method ◽  
In Vitro Dissolution ◽  
Dissolution Studies ◽  
Rp Hplc ◽  
Tablet Dosage

scholarly journals Selective Determination of Diazinon and Chlorpyrifos in the Presence of Their Degradation Products: Application to Environmental Samples

2018 ◽  
Vol 101 (4) ◽  
pp. 1191-1197 ◽  
Author(s):  
Mamdouh R Rezk ◽  
Abd El-Aziz B Abd El-Aleem ◽  
Shaban M Khalile ◽  
Omneya K El-Naggar
Keyword(s):  
Flow Rate ◽  
Environmental Samples ◽  
Mobile Phase ◽  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Uv Detection ◽  
Selective Determination ◽  
International Conference

Abstract An accurate, sensitive, and selective HPLC method was developed and validated for the determination of diazinon and chlorpyrifos. These pesticides were subjected to different stress conditions, such as acidic, alkaline, oxidative, thermal, and photolytic hydrolysis. The proposed method used a C18 Eclipse Plus column (100 × 4.6 mm, 3.5 µm) and a mobile phase consisting of acetonitrile–water (70 + 30, v/v) in an isocratic separation mode. The flow rate was 1.5 mL/min, with UV detection at 247 and 230 nm for diazinon and chlorpyrifos, respectively. The proposed method was linear over the range of 0.40–50.00 µg/mL for diazinon and 0.40–40.00 µg/mL for chlorpyrifos. The proposed method was validated per International Conference on Harmonization guidelines and subsequently applied for the successful determination of the studied pesticides in bulk form in their commercial samples in the presence of their degradation products. The developed method was used for the determination of the residues of these pesticides in lavender and rosemary leaves that were pretreated with the recommended doses of these pesticides.

scholarly journals Multivariate optimization of liquid chromatographic conditions for determination of dapagliflozin and saxagliptin, application to an in vitro dissolution and stability studies

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Sunitha Gurrala ◽  
Shiva Raj ◽  
C. V. S. Subrahmanyam ◽  
Panikumar D. Anumolu
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
In Vitro Dissolution ◽  
Simultaneous Estimation ◽  
Stability Studies ◽  
Experimental Conditions ◽  
Pharmaceutical Dosage Form

Abstract Background Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of dapagliflozin and saxagliptin in pharmaceutical dosage form. Response surface methodology was employed for optimization of experimental conditions using three factors such as organic phase (%), pH of aqueous phase, and flow rate of mobile phase. Results Virtuous separation of analytes was achieved with mobile phase consisted of acetonitrile: phosphate buffer, pH 5.8 (26:74% v/v) with flow rate 0.96 mL/min using SPOLAR C18 column (250 × 4.6 mm, 5 μ) with run time 6 min and UV detection at 236 nm. Retention time for dapagliflozin and saxagliptin were found to be 3.5 and 5.0 min, respectively. Method was validated as per ICH guidelines. The plot between peak area vs concentration for dapagliflozin and saxagliptin were rectilinear in the range of 0.2-300 μg/mL and 0.1-150 μg/mL respectively with detection and quantification limits were 0.061 and 0.18 μg/mL for dapagliflozin and 0.014 and 0.043 μg/mL for saxagliptin, respectively. Conclusion The proposed method was exploited for assay, in vitro dissolution, and stability studies of target drugs in marketed dosage form.

scholarly journals SIMPLE LIQUID CHROMATOGRAPHY METHOD WITH UV DETECTION FOR DETERMINATION OF BROMAZEPAM IN SOLID PHARMACEUTICAL DOSAGE FORMS

2019 ◽  
Vol 31 (4) ◽  
pp. 1045-1050
Author(s):  
Irena Brcina ◽  
Marija Darkovska Serafimovska ◽  
Tijana Serafimovska ◽  
Trajan Balkanov ◽  
Biljana Gjorgjeska
Keyword(s):  
Retention Time ◽  
Direct Determination ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detection ◽  
In Vitro Dissolution ◽  
Dissolution Test ◽  
Pharmaceutical Dosage Forms

Bromazepam is a psychoactive drug belonging to class of benzodiazepines with well-known hypnotic and sedative effects. It acts on the central neural system as an inhibitor of the neurotransmitter gamma aminobutyric acid. It is frequently prescribed for treatment of severe anxiety, to reduce tension, agitation and depression. Dissolution testing (the process by which a solid solute enters in to a solution) is a requirement for all solid oral dosage forms and is used in all phases of research and development for product release and stability testing. Tablet dissolution test is a standardized method for measuring the rate of drug release from a dosage form and it simulates the percentage of active substance that can be absorbed into the blood circulation. The direct determination of Bromazepam in pharmaceutical dosage forms using HPLC with UV detector to carry out dissolution test, have not yet been described. Development of HPLC method with UV detection for direct determination of in-vitro dissolution test of Bromazepam tablets, which can be used in the same time as method for determination of assay of Bromazepam in Bromazepam tablets, can make analytical procedure easier and quicker. A simple, selective, linear, precise and accurate RP-HPLC method has been developed and validated for assay and in-vitro dissolution test of Bromazepam tablets. The method was validated according to the guidelines set by the International Conference of Harmonization for validation of analytical procedures. The chromatographic separation was carried out using reversed phase HPLC LiChrospher RP Select B column (125 x 4.0 mm i.d.; 5μm) at temperature of 50oC. Mobile phase was consisting of the mixture of methanol, acetonitrile and potassium dihydrogen phosphate buffer (pH 7.0, adjusted with 0.5M Potassium hydroxide), with the ratio of 45:5:50 (v/v/v) and flow rate of 1.0 ml/min. The detection was carried out at 239 nm. System suitability tests were performed through evaluation of different parameters (retention time, tailing factor, retention factor and selectivity) on freshly prepared standard solution of bromazepam. The retention time of bromazepam in 0,1M HCl was 3.5 min. High percentage of recovery shows that the method is free from the interferences from excipients in test samples. Linearity of response was calculated as a ratio of peak areas of bromazepam vs. concentration in 0,1M HCl and spiked tablets in the concentration range of 0.0018 – 0.016 mgmL-1. The response was linear over the concentration range of 0.0018 – 0.016 mgmL-1 and coefficient of correlation was greater than 0.99. Good linearity shows that the proposed method may be useful for quickly and routinely determination of the percentage of dissolved bromazepam from bromazepam tablets and it can be a method of choice for assay determination in the same time.

Selective LC determination of cabergoline in the bulk drug and in tablets: In vitro dissolution studies

2007 ◽  
Vol 65 (9-10) ◽  
pp. 561-567
Author(s):  
A ONAL ◽  
O SAGIRLI ◽  
D SENSOY
Keyword(s):  
In Vitro Dissolution ◽  
Dissolution Studies ◽  
Bulk Drug

scholarly journals Box-Behnken Assisted Validation and Optimization of an RP-HPLC Method for Simultaneous Determination of Domperidone and Lansoprazole

Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Box Behnken Design ◽  
Rp Hplc ◽  
System Suitability ◽  
Method Optimization ◽  
Key Variables

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

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