Abstract:A simple, rapid and efficient method has been developed and validated using ultra UPLC combined with Q-ToF MS system for recognition and characterization of forced degradation products obtained from dofetilide degradation studies. The dofetilide drug is an antiarrhythmic and belongs to Class III and it was treated with various stress conditions like acidic, basic, oxidative, photolytic and thermal conditions as per ICH guidelines. The main drug shows extensive degradation towards oxidative degradation conditio… Show more
“…The parameters set for MS studies were as follows: cone voltage: 3.0 v, capillary voltage: 3.2 v, source temperature: 100 8C, desolvation temperature: 250 8C and gas flow: 800 L h À1 . Masslynx 4.1 software was used for data acquisition [15][16][17][18][19].…”
Section: Instrumentationmentioning
confidence: 99%
“…Moreover, UPLC is a common laboratory technique that decreases the cost of designing and validating a method while increasing the efficiency of analysis. The speed of separation and efficiency improve with UPLC, resulting in the rapid development of techniques [13][14][15][16][17][18][19]. The goal of ultra-performance liquid chromatography (UPLC) drug analysis is to authenticate a drug's identity and provide quantitative data, as well as to follow the progress of a disease's treatment [8].…”
A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.
“…The parameters set for MS studies were as follows: cone voltage: 3.0 v, capillary voltage: 3.2 v, source temperature: 100 8C, desolvation temperature: 250 8C and gas flow: 800 L h À1 . Masslynx 4.1 software was used for data acquisition [15][16][17][18][19].…”
Section: Instrumentationmentioning
confidence: 99%
“…Moreover, UPLC is a common laboratory technique that decreases the cost of designing and validating a method while increasing the efficiency of analysis. The speed of separation and efficiency improve with UPLC, resulting in the rapid development of techniques [13][14][15][16][17][18][19]. The goal of ultra-performance liquid chromatography (UPLC) drug analysis is to authenticate a drug's identity and provide quantitative data, as well as to follow the progress of a disease's treatment [8].…”
A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.
This work portrays the development and validation of a simple and fast UHPLC method for the
simultaneous estimation of eight bronchodilators in the drug substance. Process and performance
capability (Cpk, Ppk, PPM) studies were conducted by which it may easily conclude how well developed
method meeting the requirements. Integration of quality by design (QbD) concept to analytical method
development was also discussed. The temperature and mobile phase interaction on chromatographic
separation were studied using design of experiments (DoE). Using the QbD and design of experiments
(DoE) as combination, a design space was established for developed method. The developed method
facilitates the quantitative determination of clenbuterol hydrochloride, fluticasone, formoterol,
glycopyrrolate, levalbuterol, metaproterenol, salmeterol and theophylline as a drug substance. All the
compounds were separated within 20 min using analytical column X-Bridge BEH C18; (100 × 2.1
mm, 2.5 μ) mobile phase consisted variable mixtures of mobile phase A (10 mM ammonium acetate
pH 4.5) and mobile phase B (methanol) with the gradient elution, column temperature 30 ºC, mobile
phase flow rate 0.2 mL min/min, wavelength of detection 234 nm.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.