scholarly journals DEVELOPMENT AND VALIDATION OF RAPID STABILITY-INDICATING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF LINAGLIPTIN AND EMPAGLIFLOZIN IN PURE AND DOSAGE FORMS

2020 ◽  
pp. 172-177
Author(s):  
RAGAA EL SHEIKH ◽  
WAFAA S HASSAN ◽  
EMANH YOUSSEF ◽  
ABDULRAHMAN Y HAMDI ◽  
NAIF AHMED BADAHDAH ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Correlation Coefficient ◽  
High Performance ◽  
Dosage Forms ◽  
Hplc Method ◽  
Limits Of Detection ◽  
Stability Indicating ◽  
Tablet Dosage

Objective: A new, simple, rapid, sensitive, and accurate stability-indicating high-performance liquid chromatography (HPLC) method was developed and validated for the quantitative determination of linagliptin (LNG) and empagliflozin (EMP) in pure and tablet dosage forms. Methods: An isocratic HPLC method, using a C18 reversed-phase column (150 mm×4.6 mm i.d., particle size 5 μm) with an isocratic binary mobile phase consisting of phosphate buffer and acetonitrile (65:35, v/v), was investigated to separate the drug from its stress degradation products. The flow rate was 1.0 mL/min at ambient temperature and photodiode array detector is used at 226 nm for detection. The developed method was validated for system suitability, linearity, accuracy, precision, limits of detection and quantitation, specificity, stability, and robustness. Results: The retention time of LNG and EMP was found to be 3.276±0.002 and 6.966±0.0006 min, respectively. The calibration curve was found to be linear with the equation y=158926.39X+11.139, with a correlation coefficient of R2=0.9991 for LNG and y=22688.45X+4.259, with a correlation coefficient of R2=0.9994 for EMP over a concentration range of 2.5–7.5 μg/mL and 5.0–15 μg/mL for LNG and EMP, respectively. The limits of detection were 0.29 and 0.48 μg/mL for LNG and EMP, respectively, and the limits of quantification were 0.89 and 1.5 μg/mL for LNG and EMP, respectively. The recovery values of this method are 101.11% and 101.48% for LNG and EMP, respectively, and the reproducibility is within 0.070 and 0.277 for LNG and EMP, respectively. Conclusion: The proposed method is a rapid stability-indicating HPLC method that can be applied for the determination of LNG and EMP in pure and tablet dosage forms.

scholarly journals A new stability-indicating RP-HPLC method for the determination of dicyclomine hydrochloride and dimethicone combination in tablet dosage forms

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
J. Saroja ◽  
Anantha Lakshmi P.V. ◽  
Y. Rammohan ◽  
D. Divya Reddy
Keyword(s):  
Liquid Chromatography ◽  
Dosage Forms ◽  
Flow Speed ◽  
Hplc Method ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Rp Hplc ◽  
Tablet Formulations ◽  
Tablet Dosage

Abstract Background We describe a “stability-indicating liquid chromatography” technique for the estimation of dimethicone (DEC) and dicyclomine hydrochloride (DEH) in the established tablet formulations. Individual quantification of DEH and DEC was reported. But simultaneous quantification of DEH and DEC was lacking. DEH and DEC were analysed on an “XTerra C18 column (250 mm × 4.6 mm, 5 μm)” with the mobile phase solvent run isocratically with 0.1M K2HPO4-acetonitrile (55:45, v/v) on a flow speed of 1.0 mL/min. Results The chromatographic run period for the DEC and DEH assay was 6.0 min with retention times of 2.134 and 2.865 min, respectively. The method was validated for accuracy (99.453 to 100.417% and 99.703 to 100.303% recovery values for DEH and DEC, respectively), precision (RSV value 0.135% for DEC and 0.171% for DEH), linearity (5–15 μg/mL for DEH and 20–60 μg/mL for DEC), selectivity (no hinderance from excipients) and specificity (no hinderance from degradants) recovery. Conclusion The developed stability-indicating liquid chromatography process was well applied to established tablet formulations.

scholarly journals ANALYITCAL METHOD DEVELOPMENT AND VALIDATION OF A REVERSED-PHASE HIGHPERFORMANCE LIQUID CHROMATOGRAPHY FOR THE DETERMINATION OF MODAFINIL IN BULK AND PHARMACEUTICAL DOSAGE FORMS

2016 ◽  
Vol 9 (5) ◽  
pp. 177
Author(s):  
Bijithra Cholaraja ◽  
Shanmugasundaram P ◽  
Ragan G ◽  
Sankar Ask ◽  
Sumithra M
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Rp Hplc ◽  
Development And Validation

ABSTRACTObjective: To development and validation of a reversed-phase high-performance liquid chromatography (RP-HPLC) for the determination of modafinilin bulk and pharmaceutical dosage forms.Methods: A simple, precise, rapid, and accurate RP-HPLC method was developed for the estimation of modafinil in bulk and pharmaceutical dosageforms. Xterra RP 18 (250 mm × 4.6 mm, 5 µ particle size) with a mobile phase consisting of methanol:water 70:30 V/V was used. The flow rate1.0 ml/min and the effluents were monitored at 260 nm. The retention time and recovery time was 12 minutes. The detector response was linear inthe concentration of 10-50 µg/ml. The respective linear regression equation being Y=452.1x+65237. The limit of detection and limit of quantificationwere 4.547 and 1.377 mcg, respectively. The method was validated by determining its accuracy, precision, and system suitability.Result: The objective of the present work is to develop simple, precise, and reliable HPLC method for the analysis of modafinil in bulk andpharmaceutical dosage forms. This is achieved using the most commonly employed Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size) columndetection at 260 nm. The present method was validated according to ICH guidelines.Conclusion: In this study, a simple, fast and reliable HPLC method was developed and validated for the determination of modafinil in pharmaceuticalformulations.Keywords: Modafinil, Reversed-phase high-performance liquid chromatography, Estimation, ICH guidelines, Tablets. 

scholarly journals High performance liquid chromatography for simultaneous determination of xipamide, triamterene and hydrochlorothiazide in bulk drug samples and dosage forms

2016 ◽  
Vol 66 (1) ◽  
pp. 109-118 ◽  
Author(s):  
Soad S. Abd El-Hay ◽  
Hisham Hashem ◽  
Ayman A. Gouda
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Temperature Detection ◽  
Bulk Drug

Abstract A novel, simple and robust high-performance liquid chromatography (HPLC) method was developed and validated for simultaneous determination of xipamide (XIP), triamterene (TRI) and hydrochlorothiazide (HCT) in their bulk powders and dosage forms. Chromatographic separation was carried out in less than two minutes. The separation was performed on a RP C-18 stationary phase with an isocratic elution system consisting of 0.03 mol L−1 orthophosphoric acid (pH 2.3) and acetonitrile (ACN) as the mobile phase in the ratio of 50:50, at 2.0 mL min−1 flow rate at room temperature. Detection was performed at 220 nm. Validation was performed concerning system suitability, limits of detection and quantitation, accuracy, precision, linearity and robustness. Calibration curves were rectilinear over the range of 0.195–100 μg mL−1 for all the drugs studied. Recovery values were 99.9, 99.6 and 99.0 % for XIP, TRI and HCT, respectively. The method was applied to simultaneous determination of the studied analytes in their pharmaceutical dosage forms.

scholarly journals Validated Stability – Indicating Methods for Determination of Sofosbuvir by UPLC and HPTLC in Pure Form and Tablet Dosage Forms

2019 ◽  
pp. 1-13
Author(s):  
Sawsan A. Abdel-Razeq ◽  
Zeinab Adel Nasr ◽  
Noha S. Said
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
High Performance ◽  
Good Accuracy ◽  
Degradation Products ◽  
Dosage Forms ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Tablet Dosage

Aims: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of sofosbuvir in presence of its degradation products. Study Design: Ultra high performance liquid chromatography (UPLC), High performance thin layer chromatography (HPTLC) are developed for determination of sofosbuvir in presence of its degradation products, laboratory-prepared mixtures and in tablet dosage forms. Place and Duration of Study: Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al-Azhar University, between August 2018 and March 2019. Methodology: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of Sofosbuvir in presence of its degradation products. The first method was an Ultra Performance Liquid Chromatography (UPLC) method, in which efficient separation was carried out on phenomenex kinetex 2.6 μm C18 100 A column using a mobile phase consisting of filtered and degassed mixture of 0.1% ortho-phosphoric acid in water and methanol with the ratio of (40:60% v/v) adjusted to pH 3.5, at a flow rate of 1 mL min-1 and UV detection at 260 nm at ambient temperature. The second method is a high performance- thin layer chromatographic one (HPTLC) in which chromatographic separation was performed on silica gel 60 F254 plates, with methanol – chloroform – ammonia (2.5: 6: 1.5 % v/v/v) as a developing system followed by densitometric determination at 261 nm. Sofosbuvir was subjected to stress conditions including alkaline, acidic and oxidative degradation. Results: Beer’s law was obeyed over the range of 1-20 μg mL–1 for UPLC and 2-12 μg / spot for HPTC with good accuracy and precision using the two procedures, respectively. Results obtained was statistically analysed and found to be in accordance with those given by the reported method. Conclusion: The proposed methods were successfully applied for the determination of sofosbuvir in bulk powder, laboratory prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The methods were validated according to ICH guidelines. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE ESTIMATION OF LEDIPASVIR IN BULK AND TABLET DOSAGE FORM

2019 ◽  
pp. 326-331
Author(s):  
MINAL R GHANTE ◽  
SANJAY D SAWANT ◽  
AMOLDEEP SHINDE ◽  
SHITAL GODSE ◽  
VANDANA S NIKAM
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

Objective: The objective of this study was to develop a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the estimation of ledipasvir (LDP) in bulk and tablet formulation. Methods: Stability-indicating RP-HPLC method was developed and validated for the estimation of LDP in bulk and tablet formulation. RP-HPLC was carried out on HiQ SiL C18 columns (250 mm × 4.6 mm, 5 μ particle size) using mobile phase acetonitrile:1 mM ammonium acetate buffer in the ratio of 90:10 v/v at a flow rate of 1 ml/min. The analytes were monitored using MD 2010 PDA detector at 333 nm. Results: The retention time was found to be 3.843 min. The proposed method was found to be having linearity in the concentration range of 5–30 μg/ml. The number of theoretical plates obtained was 4236.50 which indicate the efficient performance of the column. The limit of detection was 0.305 μg/ml and limit of quantification was 0.923 μg/ml, which indicate the sensitivity of the method; the high percentage recovery indicates that the proposed method is highly accurate. The developed method has been validated according to the ICH guidelines and found to be simple, specific, precise, and accurate. Conclusion: The proposed method is precise, accurate, and stability indicating. Therefore, the proposed method can be used for routine quality control and analysis of LDP during stability studies in bulk samples and tablet dosage forms.

scholarly journals Development and validation of a single HPLC method for the determination of thirteen pharmaceuticals in bulk and tablet dosage form

2021 ◽  
Vol 35 (1) ◽  
pp. 17-31
Author(s):  
B. Tegegne ◽  
B. S. Chandravanshi ◽  
F. Zewge ◽  
L. Pillay ◽  
L. Chimuka
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Tablet Dosage

The aim of this study was to develop and validate a high performance liquid chromatography (HPLC) method for the determination of thirteen selected pharmaceutical compounds (metformin, amoxicillin, chloroquine, theophylline, trimethoprim, caffeine, norfloxacin, ciprofloxacin, acetylsalicylic acid, doxycycline hyclate, metronidazole, albendazole and cloxacillin) in bulk and tablet dosage form. Chromatographic separation using a Kromasil C18 column, gradient elution with aqueous formic acid (0.1%), methanol and acetonitrile, a UV absorption wavelength of 250 nm and a mobile phase flow rate of 1 mL/min over a 22 min run time was optimized for complete separation of the selected target compounds. The method was validated and results for: linearity, precision, sensitivity, accuracy, specificity, suitability and method robustness were obtained and met the ICH guidelines. Calibration curve correlation coefficients ranged from 0.9985-0.9998 and the percentage relative standard deviations for repeated analysis was below 5%, indicating acceptable method precision. The limits of detection (LODs) and quantification (LOQs) ranged from 0.020-0.27 µg/L and 0.080-0.91 µg/L, respectively. The accuracy study yielded recoveries in the ranges 86.0-102% for pure compounds and 90.9-106% for compounds in tablet dosage form. The method is robust for small or deliberate changes to the chromatographic parameters and found to be appropriate for analysis of tablets for the determination of the thirteen pharmaceuticals.                     KEY WORDS: Pharmaceuticals, Bulk determination, Tablet dosage, High performance liquid chromatography, Method development, ICH guidelines   Bull. Chem. Soc. Ethiop. 2021, 35(1), 17-31. DOI: https://dx.doi.org/10.4314/bcse.v35i1.2

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

Sign in / Sign up

Export Citation Format

Share Document