scholarly journals Development and validation of Stability Indicating HPLC method for estimation of Embelin in Embelia tsjeriam cottam(Vidanga)

2015 ◽  
Vol 6 (3) ◽  
Author(s):  
Sweta V Kulkarni ◽  
Mrinalini C Damle
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Good Recovery ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stress Degradation ◽  
Development And Validation ◽  
Insight Into

           Embelin, is an active phytoconstituent obtained from fruits of Embelia tsjeriam cottam, commonly known as Vidanga. A simple stability indicating HPLC method for the estimation of Embelin has been developed and validated as per ICH Q2A(R1). Sample was eluted using HiQsil C8 (4.6mm×250mm) column. The mobile phase consisted of Methanol: Acetonitrile: 1% O-phospheric acid in water in the ratio of 70:15:15 v/v/v which was sonicated to degas and delivered at a flow rate of 1ml/min at ambient temperature. The retention time of Embelin was 6.05 ± 0.2 minutes. Studies were performed using an HPLC system equipped with a UV detector; the response was monitored at 291 nm. A good linear relationship over the range of 2–10 µg/ml concentrations with correlation coefficient value of 0.999 was obtained. The accuracy of the method is indicated by good recovery in the range of 98.9-101.2 % and precision less than 2% RSD. The limit of detection and limit of quantification were found to be 0.47 and 1.44µg/ml respectively. Embelin was subjected to stress conditions as per ICH Q2A(R2) and a significant degradation was found to occur by acid hydrolysis, oxidation and thermal stress. Stress degradation studies on embelin provide an insight into its stability. 

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING METHOD RP-HPLC METHOD OF ACOTIAMIDE

2018 ◽  
Vol 10 (9) ◽  
pp. 1 ◽  
Author(s):  
Charu P. Pandya ◽  
Sadhana J. Rajput
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Acid And Base ◽  
Stress Degradation ◽  
Development And Validation ◽  
Tablet Dosage

Objective: The objective of present work was to develop and validate simple, precise, accurate and specific stability indicating method for determination of acotiamide in presence of its degradation products.Methods: An isocratic RP-HPLC method has been developed using C-8 Thermo Hypersil BDS Column (250 x 4.6 mm i.d., 5µparticle size) with the mobile phase composition of acetonitrile: 0.1 % triethylamine in 0.2% formic acid (30: 70) at column oven temperature of 40 °C. The flow rate was 1.0 ml min-1 and effluent was detected at 282 nm. The method was validated in terms of linearity, accuracy, precision, LOD (Limit of Detection), LOQ (Limit of Quantification) and robustness as per ICH guidelines.Results: The method was found to be linear in the range of 10-60µg/ml. Limit of detection and limit of quantification was found to 0.36µg/ml and 1.10 µg/ml.% Recovery was found to be in the range of 99.45%-99.75%and precision less than 2%. The developed method was successfully applied for estimation of Acotiamide in marketed tablet formulation and percentage assay was found to be 100.45%. Acotiamide was subjected to stress degradation under acid, base, neutral hydrolysis, oxidation, dry heat, photolysis conditions. Significant degradation was observed in acid and base degradation.Conclusion: The developed RP-HPLC method was simple, rapid, accurate, precise and stability indicating for the estimation of Acotiamide in bulk and tablet dosage form.

scholarly journals Development and validation of Stability Indicating HPLC method for determination of Ellagic and Gallic acid in Jambul seed

2015 ◽  
Vol 3 (3) ◽  
pp. 434-438 ◽  
Author(s):  
Mrinalini Damle ◽  
Nilam Dalavi
Keyword(s):  
Gallic Acid ◽  
Ellagic Acid ◽  
Limit Of Detection ◽  
Ethanolic Extract ◽  
Hplc Method ◽  
Uv Detector ◽  
Stability Indicating ◽  
Stress Degradation ◽  
Development And Validation

Ellagic and Gallic acid are main phytoconstituents of S.cumini seeds. These are the phenolic compounds. An approach for the stress degradation was successfully applied for the development of stability indicating HPLC method for the determination of Ellagic and Gallic acid. Sample was resolved on a Hypersil C18 (250*4.6 mm particle size 5?) column. The mobile phase consisted of 1% OPA and ACN and in the ratio of 70:30 v/v which was sonicated to degas and delivered at a flow rate of 1ml/min at ambient temperature. The retention time of Ellagic acid and Gallic acid was 3.1±0.05 & 4.1±0.05 minutes. Studies were performed using an HPLC system equipped with a UV detector; the response was monitored at 271nm. The method is specific to Ellagic and Gallic acid; it is able to resolve the peak from ethanolic extract of s.cumini seeds and formulation. The calibration curve was linear over the concentration range of 8-24 ?g/ml (r2=0.997, 0.998 resp). The limit of detection for  Ellagic acid and Gallic acid   was found to be 0.25?g/ml, 0.15?g/ml resp. and the quantification limit was about 0.75?g/m, 0.49?g/ml. The accuracy of the method was established based on the recovery studies. The markers were subjected to acid, base, neutral hydrolysis, oxidation, thermal degradation and photolysis. The method was successfully validated according to ICH guidelines Q2 (R1).Int J Appl Sci Biotechnol, Vol 3(3): 434-438

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

A new stability indicating chiral RP-HPLC method for determination of degradation products in Meclizine Hydrochloride

2020 ◽  
Vol 16 ◽  
Author(s):  
Bryan Gowramma ◽  
Ramachandran Senthil Kumar ◽  
Kaviarasan Lakshmanan ◽  
Rajagopal Kalirajan ◽  
Subramanian Nainar Meyyanathan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Stress Conditions ◽  
Main Peak ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Degradation Behaviour ◽  
Stability Indicating

Background: An enantiomeric separation of stability-indicating high-performance liquid chromatographic method was developed and validated for the analysis of Meclizine enantiomers. The degradation behaviour of Meclizine Hydrochloride was investigated under different stress conditions recommended by International Conference on Harmonization (ICH). Experiment: Enantiomeric resolution of the drug and complete separation from its degradation products were successfully achieved on a Phenomenex® lux cellulose 1 C18 (250 mm × 4.6 mm i.d, 5 µm particle size) column, using UV detector at a wavelength of 230 nm, with mobile phase consisting of acetonitrile, 20mM ammonium bicarbonate at the ratio of 75:25 (v/v), and a flow rate of 1 mL/min. The drug was subjected to alkaline, acidic, neutral, oxidative and photolytic conditions in order to mimic stress conditions. Result: The degradation products were well resolved from main peak and proving the stability-indicating power of the method. The developed method provided linear responses within the concentration range 1-5 µg/mL, and regression analysis showed a correlation coefficient value (r2) of 0.999. The HPLC method was validated as per ICH guidelines with respect to specificity, precision, linearity and robustness. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.25 µg/mL and 1.00 µg/mL respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The method was highly selective, where degradation products and co formulated compounds did not interfere. The proposed method was successfully applied in pharmaceutical preparations.

scholarly journals HPLC METHOD DEVELOPMENT AND VALIDATION FOR AZITHRO-MYCIN IN ORAL SUSPENSION

2019 ◽  
pp. 7-12
Author(s):  
Alok Pratap Singh ◽  
Iti Chauhan ◽  
Snigdha Bhardwaj ◽  
Praveen Gaur ◽  
S Sadish Kumar ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Wide Range ◽  
Tract Infections ◽  
Development And Validation

Introduction: Azithro-mycin a semi-synthetic, azalide congener of erythro-mycin indicated in the treatment of respiratory tract infections. Various methods available for determination of Azithro-mycin, but HPLC are most versatile one. Objective: The present study is based on the development and validation of a rapid, simple high performance liquid chromatography (HPLC) method equipped with UV detector for quantitative analysis of Azithro-mycin (AZN) in suspension. Material and methods: The Method was performed by using Hypersil BDS-C18 (250 mm × 4.6 mm i.d.) column MS-II, with an isocratic mobile phase of methanol, acetonitrile and phosphate buffer pH 8 (60:30:10; v/v) with run time 15 minutes. The determinations were performed at a flow rate of 1.0ml/min, and UV detector set at 212 nm. Result and Discussion: The method was found to be specific with relative standard deviation (RSD) less than 2.09%. The method showed accuracy with RSD less than 1.34% and precision in repeatability with RSD less than 1.42%. The method was found to be linear over a wide range of concentration from 1.0 to 50.0 μg/mL (R2 = .995). Limit of detection and limit of quantification were found to be 14.40 ng/mL and 43.66 ng/mL respectively. Conclusion: It was advantageous to use UV detector over other methods employing electrochemical, photodiode array etc. as the detector, because of cheap and easy availability. The developed method fulfilled all validation parameters as per ICH and can be successfully applied to quantify percent drug content in marketed oral Azithro-mycin suspension.

scholarly journals DEVELOPMENT AND VALIDATION OF HPLC-DAD METHOD FOR THE DETERMINATION OF BISOPROLOL IN TABLET DOSAGE FORMS

2017 ◽  
Vol 9 (6) ◽  
pp. 54 ◽  
Author(s):  
Yuliya Kondratova ◽  
Liliya Logoyda ◽  
Yuliia Voloshko ◽  
Ahmed Abdel Megied ◽  
Dmytro Korobko ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Label Claim ◽  
Development And Validation ◽  
Tablet Dosage

Objective: A rapid, simple and sensitive RP-HPLC method was developed and validated for the determination of bisoprolol fumarate in bulk and pharmaceutical dosage form.Methods: Chromatographic separation was achieved within 2.5 min on ACQUITY Arc System, Waters Symmetry C18 column (3.9 mm i.d. X 150 mm, 5 μm particle sizes) using a mobile phase consisted of acetonitrile: phosphate buffer (25:75 v/v) in an isocratic mode at a flow rate of 1.4 ml/min. The pH of the mobile phase was adjusted to 7.0 with orthophosphoric acid and UV detection was set at 226 nm.Results: The retention time for bisoprolol fumarate was found to be 2.09 min. The proposed method was validated according to ICH guidelines with respect to linearity, specificity precision, accuracy and robustness. The limit of detection and limit of quantification are calculated and found to be 0.4825 and 1.4621 μg/ml; respectively.Conclusion: The proposed method can help research studies, quality control and routine analysis with lesser resources available. The results of the assay of pharmaceutical formulation of the developed method are highly reliable and reproducible and is in good agreement with the label claim of the medicines.Keywords: Bisoprolol, High-Performance Liquid Chromatography, Validation, ICH guidelines

scholarly journals Development and validation of novel HPLC method for the estimation of Rutin in crude hydromethanolic leaf extract of Prosopis cineraria

2018 ◽  
Vol 8 (6) ◽  
pp. 68-73
Author(s):  
Ram Singh Bishnoi ◽  
Manish Kumar ◽  
Ajay Kumar Shukla ◽  
C.P. Jain
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Prosopis Cineraria ◽  
Liquid Chromatography Method ◽  
Development And Validation

A simple, specific, accurate and precise high performance liquid chromatography method has developed for the estimation of rutin in Prosopis cineraria. The chromatographic separation was achieved by using C18 column, 150 x 4.6mm i.d., 5µ bonded phase octadecylsilane (Thermo Labs Hypersil). Mobile phase was composed of 80 parts of methanol & 20 parts of 0.05% formic acid. The pH of the mobile phase was 3.2.The retention time of rutin was found 5.7 min with 1 mL/min flow rate at ambient temperature. The estimation was performed on PDA detector at 281 nm. In this study, an excellent linearity was obtained with r2 0.999. Besides, the chromatographic peak was found sharp & symmetric. The proposed method was validated in terms of the analytical parameters such as accuracy, linearity, precision, robustness, limit of detection (LOD), limit of quantification (LOQ) were determined based on the International Conference on Harmonization (ICH) guidelines. The detector response was linear in the range of 2-10 µg/mL. The proposed method was successfully applied for the estimation of the constituents in crude extract of Prosopis cineraria. This study established a quantitative method for the determination of rutin from Prosopis cineraria.  Keywords: Prosopis cineraria, HPLC, Validation, Rutin.

scholarly journals A SIMPLE (HPLC–UV) METHOD FOR THE QUANTIFICATION OF COLCHICINE IN BULK AND ETHOSOMAL GEL NANO-FORMULATION AND ITS VALIDATION

2017 ◽  
Vol 9 (7) ◽  
pp. 72 ◽  
Author(s):  
Ibrahim M. Abdulbaqi ◽  
Yusrida Darwis ◽  
Nurzalina Abdul Karim Khan ◽  
Reem Abou Assi ◽  
Gabriel Onn Kit Loh
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Acid Oxidation ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stress Degradation

Objective: To develop and validate a stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method for the determination of colchicine in bulk and ethosomal gel nano-formulation.Methods: The chromatographic conditions were optimized using stainless steel Hypersil Gold C-18 analytical column with the dimensions of 250 mm x 4.6 mm ID x 5 µm. The mobile phase consisted of acetonitrile and ammonium acetate buffer (20 mmol/l, pH=4.85) in the ratio of 32:68 v/v. The flow rate was set at 1 ml/min and the detection wavelength was 353 nm. The column was maintained at 30 °C and the injection volume was 10 µl. The stability of colchicine in different conditions was investigated by exposing the drug to stress degradation using acid, base, oxidation, heat and light.Results: There was no interference from excipients, impurities, dissolution media or degradation products at the retention time of colchicine 5.9 min indicating the specificity of the method. The limit of detection (LOD) and the limit of quantification (LOQ) were 8.64 ng/ml and 26.17 ng/ml respectively. The drug showed good stability under heat, acid, oxidation and light, but substantial degradation was observed under alkali condition. The procedure was validated for specificity, linearity, accuracy and precision.Conclusion: A simple, rapid, specific and stability-indicating HPLC–UV method for the determination of colchicine in the pure and ethosomal gel was successfully developed. The developed method was statistically confirmed to be accurate, precise, and reproducible.

scholarly journals A Validated New Gradient Stability-Indicating LC Method for the Analysis of Doripenem in Bulk and Injection Formulation

2013 ◽  
Vol 2013 ◽  
pp. 1-9
Author(s):  
Singaram Kathirvel ◽  
Garikapati Devalarao
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Mobile Phase Flow Rate ◽  
Phase Gradient ◽  
Stability Indicating

A sensitive, precise, specific, linear, and stability-indicating gradient HPLC method was developed for the estimation of doripenem in active pharmaceutical ingredient (API) and in injectable preparations. Chromatographic separation was achieved on C18 stationary phase with a mobile phase gradient consisting of acetonitrile, methanol, and pH 5.2 phosphate buffer. The mobile phase flow rate was 0.8 mL/min, and the eluted compounds were monitored at 210 nm. The method is linear over the range of 0.335 to 76.129 µg/mL. The correlation coefficient was found to be 0.999. The numbers of theoretical plates and tailing factor for doripenem were 53021 and 0.9, respectively. Doripenem was subjected to the International Conference on Harmonization (ICH) prescribed hydrolytic (acid, base, and neutral), oxidative, photolytic, and thermal stress conditions. Among all the above-mentioned conditions, the drug was found to be stable under photolytic degradation. Peak homogeneity data for doripenem in the chromatograms from the stressed samples obtained by use of the photodiode array detector demonstrated the specificity of the method for analysis of doripenem in presence of the degradation products. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, and robustness.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

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