scholarly journals Development and Validation of Stability-Indicating RP-UPLC Method for the Determination of Methdilazine in Bulk Drug and in Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Madihalli S. Raghu ◽  
Kanakapura Basavaiah ◽  
Cijo M. Xavier ◽  
Kudige N. Prashanth
Keyword(s):  
Limit Of Detection ◽  
Bulk Sample ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Bulk Drug

A simple, precise, and accurate, and stability-indicating isocratic Ultraperformance Liquid Chromatography (UPLC) method was developed for the determination of methdilazine hydrochloride (MDH) in bulk drug and in its tablets. The use of UPLC, with a rapid 5-minute-reversed-phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for MDH, is demonstrated. The method was developed using Waters Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogenorthophosphate and 1-pentane sulphonic acid buffer of pH 4.0 and acetonitrile (60 : 40 v/v). The eluted compound was detected at 254 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–80 μg mL−1 MDH with regression coefficient () value of 0.9999. The limit of detection () was 0.2 μg mL−1 and the limit of quantification () was 0.5 μg mL−1. Forced degradation of the bulk sample was conducted in accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal, and photolytic degradations were used to assess the stability indicating power of the method. The drug was found to be stable in acidic, basic, thermal, hydrolytic, and photolytic stress conditions and showed slight degradation in oxidative stress condition.

scholarly journals A Stability Indicating UPLC Method for the Determination of Tramadol Hydrochloride: Application to Pharmaceutical Analysis

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura B. Vinay ◽  
Hosakere D. Revanasiddappa ◽  
Cijo M. Xavier ◽  
Pavagada J. Ramesh ◽  
Madihalli S. Raghu
Keyword(s):  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Tramadol Hydrochloride ◽  
Stability Indicating

The use of Ultra Performance Liquid Chromatography (UPLC), with a rapid 5-minute reversed phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for tramadol hydrochloride (TMH) is demonstrated. A simple, precise and accurate stability-indicating isocratic UPLC method was developed for the determination of TMH in bulk drug and in its tablets. The method was developed using Waters Aquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogen phosphate buffer of pH 2.8 and an equal volume of acetonitrile (60 : 40 v/v). The eluted compound was detected at 226 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–300 μg mL−1 TMH with regression coefficient (r) value of 0.9999. The limit of detection (S/N =3) was 0.08 μg mL−1 and the limit of quantification (S/N =10) was 0.2 μg mL−1. Forced degradation of the bulk sample was conducted an accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation were used to assess the stability indicating power of the method. TMH was found to degrade significantly in acidic, basic and oxidative stress conditions and stable in thermal, hydrolytic and photolytic conditions.

VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

scholarly journals DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRICMETHOD FOR QUANTITATIVE ESTIMATION OF GLIPIZIDEIN PHARMACEUTICAL DOSAGE FORM

2020 ◽  
pp. 104-107
Author(s):  
ANUJA SURYAWANSHI ◽  
AFAQUEANSARI ◽  
MALLINATH KALSHETTI
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
The Novel ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Novel Method ◽  
Bulk Drug ◽  
Development And Validation

Objective: The present work is aimed to develop a simple, rapid, selective and economical UV spectrophotometric method for quantitative determination of Glipizideinbulk and pharmaceutical dosage form. Methods: In this method Dimethyl Form amide (DMF) was used as solvent, the absorption maxima was found to be275 nm in DMF. The developed method was validated for linearity, accuracy, precision, ruggedness, robustness, LOD and LOQ in accordance with the requirements of ICH guideline. Results: The linearity was found to be 10-60 µg/ml having linear equation y=0.017x-0.006 with correlation coefficient of 0.997. The% recovery was found to be in the range of 98.7-100%. The % RSD for intra-day and inter-day precision was found to be 0.569923 and 0.40169 respectively. The limit of detection (LOD) and limit of quantification (LOQ) was found to be3.06 µg/ml and 9.27 µg/ml respectively. Conclusion: The developed method was validated as per ICH Q2(R1) guidelines. The novel method is applicable for the analysis of bulk drug in its pharmaceutical dosage form.

scholarly journals Stability-Indicating Assay for the Determination of Pentobarbital Sodium in Liquid Formulations

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Myriam Ajemni ◽  
Issa-Bella Balde ◽  
Sofiane Kabiche ◽  
Sandra Carret ◽  
Jean-Eudes Fontan ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Drug Stability ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Reliable Determination ◽  
Pentobarbital Sodium ◽  
Stability Indicating

A stability-indicating assay by reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of pentobarbital sodium in oral formulations: a drug used for infant sedation in computed tomography (CT) or magnetic resonance imaging (MRI) scan. The chromatographic separation was achieved on a reversed-phase C18 column, using isocratic elution and a detector set at 214 nm. The optimized mobile phase consisted of a 0.01 M potassium buffer pH 3 and methanol (40 : 60, v/v). The flow rate was 1.0 mL/min and the run time of analysis was 5 min. The linearity of the method was demonstrated in the range of 5 to 250 μg/mL pentobarbital sodium solution (r2= 0.999). The limit of detection and limit of quantification were 2.10 and 3.97 μg/mL, respectively. The intraday and interday precisions were less than 2.1%. Accuracy of the method ranged from 99.2 to 101.3%. Stability studies indicate that the drug is stable to sunlight and in aqueous solution. Accelerated pentobarbital sodium breakdown by strong alkaline, acidic, or oxidative stress produced noninterfering peaks. This method allows accurate and reliable determination of pentobarbital sodium for drug stability assay in pharmaceutical studies.

scholarly journals Stability-indicating liquid chromatographic method for quantification of new anti-epileptic drug lacosamide in bulk and pharmaceutical formulation

2012 ◽  
Vol 18 (1) ◽  
pp. 35-42 ◽  
Author(s):  
Usmangani Chhalotiya ◽  
Kashyap Bhatt ◽  
Dimal Shah ◽  
Sunil Baldania ◽  
Jigar Patel
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Chemical Oxidation ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Dry Heat ◽  
Alkali Hydrolysis ◽  
Liquid Chromatographic

An isocratic stability indicating reversed-phase liquid chromatographic determination was developed for the quantitative determination of lacosamide in the pharmaceutical dosage form. A Hypersil C-18, 4.5?m column with mobile phase containing acetonitrile-water (20:80, v/v) was used. The flow rate was 1.0 mL min-1 and effluents were monitored at 258 nm. The retention time of lacosamide was 8.9 min. The method was found to be linear in the concentration range of 5-100 ?g/ml and the recovery was found to be in the range of 99.15 - 100.09 %. The limit of detection and limit of quantification were found to be 2 ?g/ml and 5 ?g/ml, respectively. Lacosamide stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The drug was found to be stable to the dry heat and acidic condition attempted. The proposed method was validated and successfully applied to the estimation of lacosamide in tablet dosage forms.

scholarly journals Dual Wavelength RP-HPLC Method for Simultaneous Determination of Two Antispasmodic Drugs: An Application in Pharmaceutical and Human Serum

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Najmul Hasan ◽  
Mathurot Chaiharn ◽  
Sauleha Khan ◽  
Hira Khalid ◽  
Nawab Sher ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stress Conditions ◽  
Dual Wavelength ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Physiological Fluid

A reverse phase stability indicating HPLC method for simultaneous determination of two antispasmodic drugs in pharmaceutical parenteral dosage forms (injectable) and in serum has been developed and validated. Mobile phase ingredients consist of Acetonitrile : buffer : sulfuric acid 0.1 M (50 : 50 : 0.3 v/v/v), at flow rate 1.0 mL/min using a HibarμBondapak ODS C18column monitored at dual wavelength of 266 nm and 205 nm for phloroglucinol and trimethylphloroglucinol, respectively. The drugs were subjected to stress conditions of hydrolysis (oxidation, base, acid, and thermal degradation). Oxidation degraded the molecule drastically while there was not so much significant effect of other stress conditions. The calibration curve was linear with a correlation coefficient of 0.9999 and 0.9992 for PG and TMP, respectively. The drug recoveries fall in the range of 98.56% and 101.24% with 10 pg/mL and 33 pg/mL limit of detection and limit of quantification for both phloroglucinol and trimethylphloroglucinol. The method was validated in accordance with ICH guidelines and was applied successfully to quantify the amount of trimethylphloroglucinol and phloroglucinol in bulk, injectable form and physiological fluid. Forced degradation studies proved the stability indicating abilities of the method.

scholarly journals Stability-indicating RP-UPLC Method for Determination of Vildagliptin in Drug Substance and Its Tablet Dosage Form

2021 ◽  
pp. 139-146
Author(s):  
Kalyani Peluri ◽  
S. Rajasekaran
Keyword(s):  
Limit Of Detection ◽  
Research Work ◽  
Cost Effective ◽  
Drug Substance ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Stability Indicating ◽  
Degradation Studies

Aim: The foremost purpose of this research work is to diminish the analysis time and to establish cost effective method for estimation of Vildagliptin by RP-UPLC. Study Design: UPLC based Quantification studies. Place and Duration of Study: Department of Pharmacy, Bhagwant University, Ajmer, Rajasthan, Indiabetween June 2020 and August 2020. Methodology: A simple, responsive and precised RP-UPLC method with good robustness was developed and validated as per ICH for the analysis of Vildagliptin in drug substance and separation of degradants generated by different forced degradation conditions. Productive separation of Vildagliptin was attained by the use of Luna C18 column (100x2.6mm and 1.6µm) with a mobile phase composition of 0.1% v/v Trifluoroacetic acid and Acetonitrile in 80:20 v/v, which was pumped with 0.5 ml/min flow rate. The eluted substances were examined with PDA detector at 239nm. Stressed degradation studies were performed with proposed method to determine the percentage degradation of Vildagliptin. Results: The RT of Vildagliptin was observed at 1.56 min. The developed method was validated as per ICHQ2B and proved that the method was precise, sensitive, specific and accurate.The lowest concentration of limit of detection (0.05µg/ml) and limit of quantification(0.5µg/ml) of Vildagliptin make obvious about the sensitivity of the method. The correlation coefficient found to be 0.9997 for given range of linear concentrations. The calculated average percentage recoveries of Vildagliptin in spiked solutions were found to be in the range of 99.1-100.5. The calculated % RSD was determined to be less than 2. Determination of degradation of amount of Vildagliptin by forced degradation studies representing the stability indicating nature of the proposed method. Conclusion: The developed method said to be highly sensitive, accurate, specific and robust, therefore this method has high probability to adopt in pharmaceutical industry for regular analysis of Vildagliptin.

scholarly journals STABILITY-INDICATING REVERSED-PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS ESTIMATION OF DARUNAVIR AND RITONAVIR

2016 ◽  
pp. 66
Author(s):  
Sindu Priya Dasyam ◽  
Gowri Sankar D ◽  
Masthanamma Sk
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

<p>ABSTRACT<br />Objective: The main objective of the proposed study was to develop and validate a new stability indicating reverse phase high performance liquid<br />chromatography method for the simultaneous estimation of darunavir (DRV) and ritonavir (RTV).<br />Methods: The method was optimized using Atlantis C18 column (50 mm×4.6 mm, 5 µm, Waters Corporation, Milford, USA). Acetonitrile and water<br />were used as mobile phase in the proportion of 60:40. The flow rate was 0.8 ml/minutes and the effluent was monitored at 230 nm.<br />Results: The retention time of DRV and RTV was 3.15 minutes and 4.59 minutes, respectively. The method was precise as it showed a % relative<br />standard deviation of &lt;2%. The percentage recoveries of both the drugs DRV and RTV were 99.8-100.01% and 99.5-99.97%, respectively. The<br />linearity of DRV and RTV was in the range of 40-120 and 4-20 µg/ml, respectively. Calibration curve showed good linearity and range. The correlation<br />coefficient of DRV and RTV was 0.999 each. Moreover, the results obtained for limit of quantification, limit of detection, robustness, and ruggedness<br />were well within the acceptance criteria.<br />Conclusion: The proposed method was found to be simple, rapid, accurate, precise, and stability indicating. It was found to be economical and suitable<br />for simultaneous determination of DRV and RTV which is can also be applied for pharmaceutical dosage form.<br />Keywords: Darunavir, Ritonavir, Reversed-phase-high performance liquid chromatography, Simultaneous estimation, Forced degradation.</p>

scholarly journals DEVELOPMENT OF A NEW STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF EPALRESTAT AND PREGABALIN AND ITS VALIDATION AS PER INTERNATIONAL CONFERENCE ON HARMONIZATION GUIDELINES

2018 ◽  
Vol 11 (5) ◽  
pp. 319
Author(s):  
Swapna Goday ◽  
Abdul Rahaman Sk ◽  
Prameelarani A
Keyword(s):  
Retention Time ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
International Conference ◽  
Stability Indicating

Objective: The present study was aimed to develop a novel, simple, rapid, accurate, stability-indicating reversed-phase high-performance liquid chromatography method, and validate for the simultaneous estimation of epalrestat and pregabalin in bulk and dosage form. Methods: The chromatographic separation was performed on c18 column discovery (250 mm × 4.6 mm, 5 μ particle size) the optimized mobile phase consists of 0.01 m potassium dihydrogen phosphate buffer: Methanol (25:75% v/v) with a flow rate of 1.0 ml/min and ultraviolet (UV) detection at 226 nm. Results: The chromatographic condition, retention time was 2.2 min (pregabalin), 2.8 min (epalrestat). Stress testing was performed in accordance with an International Conference on Harmonization (ICH) Q1A R2 guidelines. The method was validated as per ICH Q2 R1 guidelines. Linearity range was 30–180 ppm (epalrestat), 15–90 ppm (pregabalin), accuracy was in the range of 98.14–100.43% for both the drugs. Precision was 0.2% and 0.3% for epalrestat and pregabalin. Limit of detection and limit of quantification are 0.21 μg/ml and 0.65 μg/ml for epalrestat and 0.08 μg/ml and 0.25 μg/ml for pregabalin. Conclusion: The method developed is more sensitive, accurate, and precise than the methods reported earlier. Retention time and runtime were also less, and hence, the method is economical. When applied for tablet assay, drug content was within 100.06–100.22% of the labeled content. Forced degradation studies indicated the suitability of the method for stability studies. The proposed method can be used for routine determination of epalrestat and pregabalin.

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.

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