Development and Validation of a Reversed-Phase Ultra-Performance Liquid Chromatographic Method for Assay of Lacidipine and Related Substances

2011 ◽  
Vol 94 (6) ◽  
pp. 1800-1806 ◽  
Author(s):  
Arivozhi Mohan ◽  
Hitesh B Patel ◽  
Dhandayutham Saravanan
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Reversed Phase ◽  
Drug Substance ◽  
Forced Degradation ◽  
Related Substances ◽  
Forced Degradation Studies ◽  
Acetic Acid Buffer ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract A simple isocratic, RP-ultra-performance LC method was developed and validated for the determination of lacidipine, three process impurities formed during synthesis, and three degradation products present in drug substance and the drug product. An efficient chromatographic separation was achieved on an Acquity BEH C18 column using pH 4.5 ammonium acetate–acetic acid buffer–methanol (70 + 30, v/v) mobile phase. The monitoring wavelength was 240 nm, and the flow rate 0.25 mL/min. Forced degradation studies using acid, alkali, peroxide, water, heat, and light were conducted, and all impurities were separated. The method was validated successfully for specificity, precision, linearity, accuracy, LOD, LOQ, and robustness, according to International Conference on Harmonization guidelines. The linearity of the calibration curve for lacidipine and each impurity was found to be very good (r2 > 0.999). This method is shown to be suitable for analysis of lacidipine to evaluate the quality of drug substance and a drug product.

scholarly journals Determination of Mesalamine Related Impurities from Drug Product by Reversed Phase Validated UPLC Method

2011 ◽  
Vol 8 (1) ◽  
pp. 131-148 ◽  
Author(s):  
Trivedi Rakshit Kanubhai ◽  
Patel Mukesh C ◽  
Kharkar Amit R
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Release Formulation ◽  
Delayed Release ◽  
Related Substances

In the present study gradient reversed-phase UPLC method was developed for simultaneous determination and separation of impurities and degradation products from drug product. The chromatographic separation was performed on acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 µm) using gradient elution. Other UPLC parameters which were optimised are flow rate, 0.7 mL/min; detection wavelength, 220 nm; column oven temperature, 40°C and injection volume 7 µL. Stability indicating capability was established by forced degradation experiments and separation of known degradation products. The method was validated as per International Conference on Harmonization (ICH) guideline. For all impurities and mesalamine, LOQ (limit of quantification) value was found precise with RSD (related standard daviation) of less than 2.0%. In essence, the present study provides an improved low detection limit and lower run time for evaluation of pharmaceutical quality of mesalamine delayed-release formulation. Moreover, the developed method was successfully applied for quantification of impurities and degradation products in mesalamine delayed-release formulation. The same method can also be used for determination of related substances from mesalamine drug substance.

Stability-indicating LC method for the determination of cephalothin in lyophilized powder for injection

2014 ◽  
Vol 6 (12) ◽  
pp. 4437-4445 ◽  
Author(s):  
Karen de Souza Rugani ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Liquid Chromatography ◽  
Degradation Products ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Antimicrobial Compound ◽  
Reversed Phase Liquid Chromatography ◽  
Stability Indicating ◽  
Forced Degradation Studies ◽  
Phase Liquid

A stability-indicating gradient reversed phase liquid chromatography (RP-LC) method has been developed for the quantitative determination of cephalothin (CET), an antimicrobial compound, in the presence of its impurities and degradation products generated from forced degradation studies.

scholarly journals LC-MS/MS CHARACTERIZATION OF FORCED DEGRADATION PRODUCTS OF TUCATINIB, A NOVEL TYROSINE KINASE INHIBITOR: DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD

2022 ◽  
pp. 58-66
Author(s):  
S. K. REEHANA ◽  
K. SUJANA
Keyword(s):  
Kinase Inhibitor ◽  
Degradation Products ◽  
Degradation Pathway ◽  
Hplc Method ◽  
Forced Degradation ◽  
Ich Guidelines ◽  
System Suitability ◽  
Forced Degradation Studies ◽  
Development And Validation

Objective: The current study focused on the development, validation, and characterization of forced degradation products using LC-MS/MS. Methods: A simple, selective, validated and well-defined isocratic HPLC methodology for the quantitative determination of Tucatinib at a wavelength of 239 nm. An isocratic elution of samples was performed on an Inertsil ODS (250x4.6 mm, 5m) column with a mobile phase of 70:30v/v Acetonitrile and formic acid (0.1%) delivered at a flow rate of 1.0 ml/min. MS/MS was used to characterize degradation products formed in the forced degradation study. The validation and characterization of forced degradation products were performed in accordance with ICH guidelines. Results: Over the concentration range of 5-100μg/ml, a good linear response was obtained. Tucatinib's LOD and LOQ were determined to be 0.05 and 0.5, respectively. According to standard guidelines, the method was quantitatively evaluated in terms of system suitability, linearity, precision, accuracy, and robustness, and the results were found to be within acceptable limits. The drug was degraded under acidic, alkaline, and reduction conditions in forced degradation studies. Conclusion: The method was found to be applicable for routine tucatinib analysis. Because no LC-MS/MS method for estimating tucatinib and its degradation products has been reported in the literature. There is a need to develop a method for studying the entire tucatinib degradation pathway.

scholarly journals Studies on Paliperidone in OROS Tablets: Extraction Procedure and Chromatographic Analysis

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Fábio Barbosa ◽  
Luciano Mantovani ◽  
Cássia V. Garcia ◽  
Andreas S. L. Mendez
Keyword(s):  
Oral Delivery ◽  
Degradation Products ◽  
Extraction Procedure ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Phase System ◽  
Stability Indicating ◽  
Ultrasonic Bath ◽  
The Stability ◽  
Liquid Chromatographic

A stability-indicating liquid chromatographic (LC) method was studied for the determination of paliperidone in osmotic-controlled release oral delivery system (OROS) tablets. A tablet extraction procedure was developed by testing the efficiency of solvents (water, HCl, NaOH, acetonitrile, methanol) and techniques (ultrasonic bath, magnetic stirrer), and evaluating the release of the drug with respect to time. A forced degradation study was conducted to demonstrate the stability-indicating power of the method. Chromatographic separation was achieved using an isocratic elution in a reversed-phase system with a mobile phase prepared from a mixture of phosphate buffer and acetonitrile. The use of an ultrasonic bath demonstrated paliperidone release from OROS tablets in a total time of 60 min. Verifying the efficiency of the chromatographic procedure, the theoretical plates (N=12634.21) and tailing factor (tf=1.31) were constant during repeated injections. The retention time of paliperidone was 4.8 min, and the method was validated within the concentration range of 10–50 μg mL-1 (r=0.9999). Adequate reproducibility (RSD% = 0.30–0.59), interday precision (RSD%=1.81), and accuracy were obtained. The proposed method was successfully applied to paliperidone determination in the presence of degradation products, and an efficient extraction procedure from the OROS tablets was developed.

Development and Validation of Stability-Indicating HPLC Method for Roflumilast and Related Substances

2013 ◽  
Vol 781-784 ◽  
pp. 68-71 ◽  
Author(s):  
Fang Tan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Limit Of Quantitation

A reversed phase HPLC method was developed and validated for analysis of roflumilast, its related substances and degradation products, using Ecosil C18 column (250×4.6 mm, 5 μm) with a flow rate of 1.0 ml/min and detection wavelength of 215nm. The mobile phase was a mixture of acetonitrile and 0.005mol·L-1ammonium dihydrogen phosphate buffer pH 3.5 in the ratio of 48:52 (v/v). The samples were analyzed using 20 μl injection volume and the column temperature was maintained at 30°C. The limit of detection and limit of quantitation were found to be 2.6 ng/ml and 8ng/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method is sensitive, specific, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds.

scholarly journals STABILITY INDICATING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF LABETALOL AND ITS DEGRADATION PRODUCTS IN TABLET DOSAGE FORMS

2016 ◽  
pp. 242 ◽  
Author(s):  
V. Ashok Chakravarthy ◽  
Sailaja Bbv ◽  
Praveen Kumar A
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Dosage Forms ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Liquid Chromatographic Method ◽  
Forced Degradation Studies ◽  
Tablet Dosage ◽  
Liquid Chromatographic

<p>ABSTRACT<br />Objective: The objective of the present work is to develop a simple, efficient, and reproducible stability indicating reverse phase high-performance<br />liquid chromatographic method for simultaneous determination labetalol and its degradation products in tablet dosage forms.<br />Methods: The chromatographic separation of labetalol and its degradation products in tablets was carried out on Zorbax Eclipse Plus C-18<br />(100 × 4.6 mm, 3.5 µm) column using 0.1% trifluoroacetic acid (TFA) (v/v) in 1000 ml of water and 0.1% TFA (v/v) in 1000 ml of acetonitrile:<br />Methanol (1:1) by linear gradient program. Flow rate was 1.0 mL min<br /> with a column temperature of 35°C, and detection wavelength was carried out<br />at 230 nm. Known impurity is well resolved from the main active drug within 14 minutes run time.<br />−1<br />Results: The forced degradation studies were performed on labetalol tablets under acidic, basic, oxidation, thermal, humidity, and photolytic<br />conditions. No degradation products were observed from the forced degradation studies, and the known impurity is well resolved from the main<br />active drug. The method was validated in terms of specificity, linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, and<br />robustness as per the ICH guidelines. The method was found to be linear in the range of LOQ to 120% for all the known and unknown impurities.<br />The LOD and LOQ values of known impurity were found between 0.3593 and 0.7187 µg mL<br />, and the percentage recovery values were in the range<br />of 95.5-105.2% at different concentration levels. Relative standard deviation for precision and intermediate precision results were found to be &lt;5%.<br />The correlation coefficient found for all compounds was not &lt;0.99. The results obtained from the validation experiments prove that the developed<br />method is a stability indicating method.<br />−1<br />Conclusion: The developed method can be successfully applied for routine analysis, quality control analysis and also suitable for stability analysis of<br />the simultaneous determination of labetalol and its degradation products in tablet dosage forms as per the regulatory requirements.<br />Keywords: Labetalol, Development, Validation, Reverse phase high-performance liquid chromatography.</p>

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