scholarly journals Development and Validation of a Rapid and Simple UPLC–ESI–MS Method for Pharmacokinetics and Tissue Distribution of Astragaloside III in Rats

2016 ◽  
Vol 54 (5) ◽  
pp. 811-818 ◽  
Author(s):  
Xiao-Hua Liu ◽  
Long Guo ◽  
Ying-Lai Yang ◽  
Fang Hu ◽  
Xin-Yue Chen ◽  
...  
Keyword(s):  
Tissue Distribution ◽  
Esi Ms ◽  
Development And Validation

scholarly journals UHPLC-ESI-MS/MS Quantification of Relevant Substrates and Metabolites of the Kynurenine Pathway Present in Serum and Peritoneal Fluid from Gastric Cancer Patients—Method Development and Validation

2021 ◽  
Vol 22 (13) ◽  
pp. 6972
Author(s):  
Ilona Sadok ◽  
Katarzyna Jędruchniewicz ◽  
Karol Rawicz-Pruszyński ◽  
Magdalena Staniszewska
Keyword(s):  
Gastric Cancer ◽  
Cancer Patients ◽  
Peritoneal Fluid ◽  
Method Development ◽  
Solid Phase ◽  
Kynurenine Pathway ◽  
Serum Samples ◽  
Esi Ms ◽  
Gastric Cancer Patients ◽  
Development And Validation

Metabolites and enzymes involved in the kynurenine pathway (KP) are highly promising targets for cancer treatment, including gastrointestinal tract diseases. Thus, accurate quantification of these compounds in body fluids becomes increasingly important. The aim of this study was the development and validation of the UHPLC-ESI-MS/MS methods for targeted quantification of biologically important KP substrates (tryptophan and nicotinamide) and metabolites(kynurenines) in samples of serum and peritoneal fluid from gastric cancer patients. The serum samples were simply pretreated with trichloroacetic acid to precipitate proteins. The peritoneal fluid was purified by solid-phase extraction before analysis. Validation was carried out for both matrices independently. Analysis of the samples from gastric cancer patients showed different accumulations of tryptophan and its metabolites in different biofluids of the same patient. The protocols will be used for the evaluation of tryptophan and kynurenines in blood and peritoneal fluid to determine correlation with the clinicopathological status of gastric cancer or the disease’s prognosis.

scholarly journals Simultaneous and Trace Level Determination of Six Potential Impurities by UPLC-ESI-MS/MS in Antiarrhythmic Drug: Dronedarone Hydrochloride

2020 ◽  
Vol 32 (5) ◽  
pp. 1183-1190
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Solvent Mixture ◽  
Column Temperature ◽  
Esi Ms ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Validation Tests ◽  
Development And Validation

Development and validation of six potential impurities by ultra performance liquid chromatography electro spray ionization tandem mass (UPLC-ESI-MS/MS) method for dronedarone hydrochloride drug was accomplished coherent with ICH guidelines. Successful chromatographic separation of dronedarone with its six impurities was attained by using gradient elution mode on RP-UPLC column using three pump mode system of 0.1 % formic acid in water as mobile phase A, methanol as the mobile phase B and solvent mixture of methanol, acetonitrile and water in the ratio of 65:30:5 v/v/v as the mobile phase C. Chromatographic conditions were set as 0.3 mL min-1 flow rate at the column temperature of 45 °C with the injection volume 2 μL. Briefly, the method enabled quantitation of six impurities with high accuracy (recovery > 90 %) and precision (% RSD < 5.0),within the ranges of 0.18-2.82 μg g-1. The regression (r) for each impurity over a range was > 0.99. The detection limit and quantitation limit of impurities were set at 0.09 and 0.18 μg g-1, respectively. The performed validation tests proved the suitability of the method for its intended purposes.

scholarly journals Development and Validation of UPLC-ESI-MS/MS Technique for the Determination of 2-Isopropyl-4-(chloromethyl)thiazole in Ritonavir

2020 ◽  
Vol 32 (7) ◽  
pp. 1733-1740
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  
Keyword(s):  
High Strength ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Internal Diameter ◽  
Esi Ms ◽  
Quantitation Limit ◽  
Highly Sensitive ◽  
Liquid Chromatography Tandem Mass ◽  
Development And Validation

The objective of this work was to develop and validate a rapid, highly sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-ESI-MS/MS) method for the quantification of 2-isopropyl-4-(chloromethyl)thiazole in ritonavir. Chromatographic conditions of this impurity were achieved on an AQUITY UPLC column HSS (high strength silica) T3 column (100 mm long, 2.1 mm internal diameter, 1.8 μm diameter) using a gradient elution with 0.1% formic acid in water and methanol at a flow rate of 0.3 mL/min. LCMS/MS was operated under the multiple reaction mode (MRM) using electrospray ionization technique in positive ion mode and the transitions of m/z 176.1[M+H]+→140.1 for quantifier, 176.1[M+H]+→71.0 for qualifier were used to measure the impurity, respectively. The total chromatographic run time was 10 min. Full validation of the analytical method was carried out, including its system precision, selectivity, linearity, accuracy, recovery, ruggedness, stability and robustness. A linear response function was achieved in the concentration range of 0.12-1.86 μg/g with r > 0.99. The detection limit and quantitation limit of this impurity were 0.06 and 0.12 μg/g, respectively. Consistent recoveries were obtained during intra- and inter-day precision experiments in validation ranged from 80-120%. The developed method could be helpful not only for quality control and also for risk management of potential genotoxicity of this impurity in ritonavir drug substance.

Development and validation of a LC-ESI–MS/MS method for the determination of swertiamarin in rat plasma and its application in pharmacokinetics

2011 ◽  
Vol 879 (19) ◽  
pp. 1653-1658 ◽  
Author(s):  
Hong-Liang Li ◽  
Xiao-Jin Peng ◽  
Jian-Chang He ◽  
En-Fu Feng ◽  
Gui-Li Xu ◽  
...  
Keyword(s):  
Rat Plasma ◽  
Esi Ms ◽  
Development And Validation
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