Estimation of Ceftazidime and Avibactam in their Bulk and Formulations by a newly Developed and Validated of Stability Indicating RP-UPLC Method

2021 ◽  
pp. 2459-2463
Author(s):  
Sridatla V.V.S.S.N. Raju ◽  
S. Venkat Rao ◽  
A. Manikandan
Keyword(s):  
Flow Rate ◽  
Efficient Method ◽  
Mobile Phase ◽  
Regression Equation ◽  
Stability Indicating

A delicate, fast, Accurate, exact and steadiness, showing isocratic RP-UPLC method was developed for the concurrent assurance of the Ceftazidime and Avibactam in bulk and formulation. To optimize, a column HSS C18 100 x 2.1mm, 1.8µm, Mobile phase containing water: acetonitrile choose in the ratio 75:25v/v was pumped through column at a flow rate of 0.3ml/min at 260nm, initiate to be an efficient method for elution of drug with good peak shapes as well as retention times. Rt of Avibactam and Ceftazidime were initiate to be 1.463 min and 2.109 min. %Recovery was obtained as 100.07% and 100.08% for Avibactam and Ceftazidime separately. LOD, LOQ values got from relapse conditions of Avibactam and Ceftazidime were 0.85, 2.56 and 3.53, 10.70 correspondingly. Regression equation of Ceftazidime is y = 7883.2x + 12277, and y = 3279.1x + 1137 of Avibactam.

scholarly journals A New Validated Stability Indicating RP-HPLC Method for Simultaneous Quantification of Formoterol Fumarate Dihydrate and Mometasone Furoate in Metered Dose Inhalation Aerosol

2021 ◽  
Vol 33 (11) ◽  
pp. 2723-2728
Author(s):  
Surya Prakash Mamillapalli ◽  
Gourabattina Lakshmi Prasanna ◽  
B. Venkata Subbaiah ◽  
N. Annapurna
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Mometasone Furoate ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Metered Dose ◽  
Formoterol Fumarate ◽  
Dose Inhalation

Stability indicating reversed phase-HPLC method for simultaneous estimation of mometasone furoate (MAF) and formoterol fumarate (FFD) in metered dose inhalation aerosol (MDI) dosage formulation has been developed and discussed in the present work. The chromatographic separation was achieved using Hypersil ODS column (250 mm × 4.6 mm, 3 μm) using an isocratic separation mode at a flow rate of 1.2 mL/min, column temperature of 50 ºC. The system operates with a mobile phase comprising of solution-A (buffer): Solution-B (acetonitrile) mixed in the ratio of 70:30 %v/v at a UV detection wavelength of 214 nm. Retention times of mometasone furoate and formoterol fumarate found to be about 3 min and 7 min, respectively. All possible degradation products of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector. Both analyte were subjected to force degradation studies, found all degradants were resolved from analyte peaks and also other process-related impurities. The proposed method is validated for specificity, linearity, accuracy, precision and robustness as per ICH guidelines and found to be adequate. Method stood to be robust with variation in column temperature, flow rate, pH of buffer and organic content in mobile phase.

scholarly journals Validated Stability-Indicating HPLC-UV Method for Simultaneous Determination of Glipizide and Four Impurities

2011 ◽  
Vol 94 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sakshi Gupta ◽  
Gulshan Bansal
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Stability Testing ◽  
Stability Indicating ◽  
Chromatographic Parameters ◽  
Interday Precision ◽  
Calculated Amount

Abstract A selective stability-indicating HPLC-UV method for simultaneous determination of glipizide and four impurities (DPs IIV) formed under hydrolytic conditions was developed and validated. The drug and impurities were resolved on an XTerra C18 column (250 4.5 mm id) in a single gradient run using buffer (0.005 M KH2PO4; pH 3.0)methanol (60 40, v/v; mobile phase A) and (20 80, v/v; mobile phase B) at a flow rate of 0.5 mL/min with 230 nm detection wavelength. The method was linear across concentration ranges of 0.2100, 0.1100, 0.5100, 0.2100, and 0.150 0000g/mL for glipizide and DPs IIV, respectively. The RSD for intraday and interday precision for the drug and impurities was <1 and <1.2, respectively. Satisfactory recoveries (96.5899.97) of each of the three concentrations selected across the linearity range of each analyte were obtained, proving the method was sufficiently accurate. The LOD was 0.07, 0.05, 0.16, 0.08, and 0.05 g/mL and the LOQ was 0.20, 0.14, 0.50, 0.23, and 0.14 g/mL for the drug and DPs IIV, respectively. Each peak was resolved with resolution of >2 from the nearest peak. Insignificant changes in retention time (<4) and calculated amount (<1.65) of drug and each impurity upon small but deliberate changes in various chromatographic parameters were observed, suggesting the method was robust. The method was applied successfully to stability testing of glipizide tablets.

scholarly journals Development and Validation of HPLC Fluorescence and UPLC/DAD Stability-Indicating Methods for Determination of Hepatitis C Antiviral Agent Daclatasvir

2019 ◽  
Vol 102 (4) ◽  
pp. 1125-1131
Author(s):  
Amira H Kamal ◽  
Nahla S Ismail ◽  
Mokhtar M Mabrouk ◽  
Lories I Bebawy ◽  
Mai A Mekky
Keyword(s):  
Fluorescence Detection ◽  
Flow Rate ◽  
Mobile Phase ◽  
Ammonium Phosphate ◽  
Uv Detection ◽  
Array Detector ◽  
Fragmentation Pattern ◽  
Stability Indicating ◽  
Ich Guidelines

Abstract Background: Few stability-indicating chromatographic methods were published for determination of daclatasvir. All used UV detection. Objective: This work aimed to develop rapid, specific, and novel stability-indicating methods using HPLC with fluorescence detection and ultra performance liquid chromatography (UPLC) with UV detection for the determination of daclatasvir in bulk powder and in its dosage form. Methods: The drug was subjected to hydrolysis (acidic and alkaline) as per International Conference on Harmonization (ICH) guidelines. The fragmentation pattern of the drug was studied using LC-MS. Separation was carried out first by HPLC using Thermo BDS Hypersil Phenyl (300 mm × 4 mm, 5 μm) column and a mobile phase consisting of ammonium phosphate buffer (0.02 M) pH 3–methanol (40+60, v/v) at flow rate 1 mL/min. Quantitation was achieved by fluorescence detection at 305 and 457 nm for excitation and emission, respectively. The second method used UPLC equipped with diode-array detector. Acquity BEH C18 (50 mm × 2.1 mm, 1.7 μm) column was used with the same mobile phase at flow rate 0.4 mL/min and detection wavelength at 305 nm. ICH guidelines were used for validation. Results: The mean percentage recovery ± SD values for tablet assay were found to be 101.12 ± 0.655 and 99.78 ± 0.632 by HPLC and UPLC methods, respectively. The assay results showed a good agreement with the reported method. Conclusions: The developed HPLC and UPLC methods provide simple, accurate, and reproducible analysis of daclatasvir without interference from degradates. Highlights: This is the first research using fluorescence detection in a stability-indicating chromatographic method for determination of daclatasvir.

scholarly journals Determination of Sinomenine in Cubosome Nanoparticles by HPLC Technique

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Yanfang Zhou ◽  
Chunlian Guo ◽  
Hongying Chen ◽  
Yudai Zhang ◽  
Xinsheng Peng ◽  
...  
Keyword(s):  
Quality Control ◽  
Flow Rate ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Regression Equation ◽  
Good Linearity ◽  
Hplc Technique ◽  
Perfect Recovery

We applied HPLC technique to quantitatively analyze sinomenine in cubosome nanoparticles. The chromatographic method was performed by using an isocratic system. The mobile phase was composed of methanol-PBS(pH6.8)-triethylamine (50 : 50 : 0.1%) with a flow rate of 1 mL/min; the detection wavelength was at 265 nm. Sinomenine can be successfully separated with good linearity (the regression equation is A=10835C+1058; R2=1.0) and perfect recovery (102.2%). The chromatograph technique was proper for quality control of sinomenine in cubosome nanoparticles.

Chromatographic Separation of the Novel Hypoglycemic Drug Mitiglinide in its Bulk Powder and Pharmaceutical Formulation: Forced Degradation and Validated Stability-Indicating HPTLC/Densitometry and HPLC/UV Methods

2020 ◽  
Vol 103 (3) ◽  
pp. 736-742
Author(s):  
Maya S Eissa ◽  
Eman Darweish ◽  
Mohammed R Elghobashy ◽  
Mostafa A Shehata
Keyword(s):  
Stationary Phase ◽  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Relative Standard ◽  
Hypoglycemic Drug ◽  
Hptlc Method

Abstract Background Mitiglinide (MTG) is one of meglitinides group which are used for treatment of type two diabetes mellitus. Objective Mitiglinide (MTG) is a novel oral hypoglycemic drug. The present work adopts two stability-indicating chromatographic methods for determination of MTG after being exposed to forced degradation using 4 M methanolic HCl for 12 h. Methods The first method is HPTLC/densitometry using methanol:chloroform:acetic acid (5:2.5:0.3 by volume) as the eluting system and silica gel 60 GF254 as the stationary phase; the separated bands were then scanned at 220 nm. The second method is HPLC/UV in which acetonitrile:methanol:0.05 M potassium dihydrogen orthophosphate (pH 3.5) (40:25:35 by volume) was used as the mobile phase and a Zorbax SB-C8 (250 × 4.6 mm, 5 µm) column as a stationary phase, at a flow rate of 1 mL/min and UV detection at 220 nm. Results As a result of acid hydrolysis, two degradants were obtained. The first one was benzyl succinic acid to which this study was performed. The second one lacked configuration and was unreadable using UV spectrometry. Linearity was in the range of 8–48 µg/band MTG for HPTLC and 10–80 µg MTG for HPLC. LOD and LOQ values were 1.85 and 5.62 µg/band for the HPTLC method and 2.14 and 6.49 µg/mL for the HPLC method, respectively. The Recovery % was 100.03 ± 1.464 and 99.61 ± 1.44 using the HPTLC and HPLC methods, respectively. The relative standard deviations (RSD, %) for intra- and inter-day assays were 1.111 and 1.430 for the HPTLC method, respectively, and those for the HPLC method were 1.377 and 0.866, respectively. The RSD, %, for robustness testing was 1.162 (saturation time of mobile phase) and 1.592 (change in ratio of methanol content) for the HPTLC method and 1.377 (mobile phase composition), 1.713 (detector wavelength) and 1.770 (mobile phase flow rate) for the HPLC method. Conclusions The adopted methods were successfully applied for the determination of MTG in its pure form, in presence of its acid degradant and in its tablet dosage form. Highlights Statistical comparison between the results obtained from the developed methods and those obtained by the reported HPLC method showed no significance difference.

A stability indicating RP-HPLC- PDA method for simultaneous estimation of segesterone acetate and ethinyl estradiol in tablet dosage form

2021 ◽  
Vol 25 (9) ◽  
pp. 113-117
Author(s):  
Narendra Reddy Yeragodala ◽  
Sreeramulu Jadi
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Ethinyl Estradiol ◽  
Simultaneous Estimation ◽  
Precise Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

A simple, accurate, precise method was developed for the simultaneous estimation of the Segesterone acetate and Ethinyl estradiol in a tablet dosage form. The chromatogram was run through Discovery C18 150 x 4.6mm, 5mm column and mobile phase containing buffer 0.01N KH2PO4: Acetonitrile taken in the ratio 50:50 was pumped through the column at a flow rate of 1 ml/min. The temperature was maintained at 30°C. The optimized wavelength selected was 240.0 nm. Ethinyl estradiol and Segesterone acetate were eluted at 2.348 min and 3.855 min respectively.

scholarly journals High Performance Liquid Chromatography (HPLC) Stability Indicating Method for the Determination of Bromazepam Via its Copper (II) Chelates

2017 ◽  
Vol 4 (1) ◽  
pp. 32-42 ◽  
Author(s):  
Assefa Takele ◽  
Abdel-Maaboud I. Mohamed Attaya ◽  
Ariaya Hymete ◽  
Melisew Tadele Alula
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Azomethine Nitrogen ◽  
Column Temperature ◽  
Stability Indicating ◽  
Stability Indicating Method

Introduction: Bromazepam is hydrolyzed in acidic aqueous solution leading to a series of degradation products. The rate of acidic hydrolysis is believed to be dependent on the state of protonation of the pyridyl and azomethine nitrogen atoms. Stability test is important in pharmaceutical industry to provide evidence on how the quality of an active substance or pharmaceutical product varies with time under the influence of a variety of environmental factors. Objective: The aim of the study was to develop a simple stability indicating method for the determination of bromazepam. Method: Bromazepam solution was prepared and forced degradation of bromazepam was performed under acid hydrolysis using sulphuric acid. High performance liquid chromatography determination of pure and degraded bromazepam and bromazepam-copper (II) complex was performed using reversed phase octyl C-8 column under isocratic conditions and the chromatographic conditions were set as follows; the flow rate of the mobile phase was 1.5 mL/min; injection volume was 10 μL, column temperature was 30oC and the detector wavelength being 309 nm. Results: Bromazepam, its degradation product and bromazepam chelated with copper (II) were determined using the developed mobile phase with flow rate of 1.5 mL/min. Good separation with sharp peak, minimum tailing and retention time repeatability was obtained. The rate order, rate constant and half-life of degradation were also determined, and it was observed that the degradation reaction follows the first order kinetics. Conclusion: Chromatographic separation of bromazepam chelated with copper (II) was achieved and the method can be further used in drug manufacturing quality control.

Stability indicating Analytical Method Development using Quality by Design (QbD) approach for simultaneous estimation of Ivabradine and Metoprolol

2021 ◽  
pp. 5937-5944
Author(s):  
Noopur K. Gandhi ◽  
Sindhu B. Ezhava
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Quality By Design ◽  
Reversed Phase ◽  
Fractional Factorial ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Mobile Phase Flow Rate ◽  
Stability Indicating

The applicability of a quality by design (QbD) approach for the development of a sensitive and selective stability indicating reversed-phase high performance liquid chromatography (RP-HPLC) method for the estimation of Ivabradine and Metoprolol was investigated. Design of experiments using a fractional factorial design approach was used for method development. Fifteen experimental runs were performed to optimize the chromatographic conditions like mobile phase, flow rate and column oven temperature. Mobile phase composition was optimized by changing Acetonitrile composition ranging between 13 and 17% v/v, Flow rate from 0.6 to 1.0 ml/min and temperature between 30 to 50 0C. The optimized method produced sharp peaks with good resolution (>2) for Metoprolol and Ivabradine with retention times of 3.3 and 9.2 min, respectively. The experimental data revealed that volume of Acetonitrile in mobile phase was prominently affecting the Retention time, Resolution & tailing factor of both the drugs. Normal probability plots revealed that the residual and predicted data fall approximately on a straight line, indicating that the experimental error for these studies was evenly distributed suggesting that the model could be used to navigate the design space. This approach is useful to expedite method development and optimization activities in analytical laboratories.

Development, Validation and Application of HPLC Method for Metformin in Rabbit Plasma

2019 ◽  
Vol 15 (6) ◽  
pp. 574-579
Author(s):  
Muhammad Ubaid ◽  
Mahmood Ahmad ◽  
Farhan Ahmad Khan ◽  
Ghulam Murtaza
Keyword(s):  
Flow Rate ◽  
Present Method ◽  
Mobile Phase ◽  
Hplc Method ◽  
Plasma Samples ◽  
Rabbit Plasma ◽  
Uv Detector ◽  
Reverse Phase ◽  
T Values ◽  
Pharmacokinetic Evaluation

Objective:This study was aimed at conducting a pharmacokinetic evaluation of metformin in rabbit plasma samples using rapid and sensitive HPLC method and UV detection.Methods:Acetonitrile was used for protein precipitation in the preparation of plasma samples. Reverse phase chromatography technique with silica gel column (250 mm × 4.6 mm, 5 μm) at 30°was used for the separation purpose. Methanol and phosphate buffer (pH 3.2) mixture was used as a mobile phase with flow rate 0.8 ml/min. The wavelength of UV detector was adjusted at 240 nm.Results:The calibration curve was linear in a range of 0.1-1 µg/ml with R² = 0.9982. The precision (RSD, %) values were less than 2%, whereas, accuracy of method was higher than 92.37 %. The percentage recovery values ranged between 90.14 % and 94.97 %. LOD and LOQ values were 25 ng/ml and 60 ng/ml, respectively. Cmax and AUC0-t values were found to be 1154.67 ± 243.37 ng/ml and 7281.83 ± 210.84 ng/ml.h, respectively after treating rabbits with a formulation containing 250 mg metformin.Conclusion:Based on the above findings, it can be concluded that present method is simple, precise, rapid, accurate and specific and thus, can be efficiently used for the pharmacokinetic study of metformin.

Optimum HPLC Conditions for Determination of Dibucaine HCL, Fluocortolone Pivalate and Fluocortolone Caproate by Using Experimental Design

2018 ◽  
Vol 15 (1) ◽  
pp. 32-38 ◽  
Author(s):  
Bürge Aşçı ◽  
Mesut Koç
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Acid Mixture ◽  
Solution Stability ◽  
Uv Detector

Introduction:This paper presents the development and validation of a novel, fast, sensitive and accurate high performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical preparations.Experiment:Development of the chromatographic method was based on an experimental design approach. A five-level-three-factor central composite design requiring 20 experiments in this optimization study was performed in order to evaluate the effects of three independent variances including mobile phase ratio, flow rate and amount of acid in the mobile phase.Conclusion:The optimum composition for mobile phase was found as a methanol:water:acetic acid mixture at 71.6 : 26.4 : 2 (v/v/v) ratio and optimum separation was acquired by isocratic elution with a flow rate of 1.3 mL/min. The analytes were detected using a UV detector at 240 nm. The developed method was validated in terms of linearity, precision, accuracy, limit of detection/quantitation and solution stability and successfully applied to the determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical topical formulations such as suppositories and ointments.

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