scholarly journals Simultaneous Determination of Chrysin and Tectochrysin from Alpinia oxyphylla Fruits by UPLC-MS/MS and Its Application to a Comparative Pharmacokinetic Study in Normal and Dementia Rats

Molecules ◽  
2018 ◽  
Vol 23 (7) ◽  
pp. 1702 ◽  
Author(s):  
Xu Zhao ◽  
Xin Su ◽  
Chunmei Liu ◽  
Ying Jia
Keyword(s):  
Simultaneous Determination ◽  
Pharmacokinetic Study ◽  
Peak Plasma ◽  
Multiple Reaction Monitoring ◽  
Peak Plasma Concentration ◽  
Area Under The Curve ◽  
Ethanol Extract ◽  
Comparative Pharmacokinetic ◽  
Alpinia Oxyphylla

A simple and rapid ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) coupled with a one-step liquid-liquid extraction method has been developed and validated for the simultaneous determination of two flavonoids (chrysin, tectochrysin) from Alpinia oxyphylla fruits extract in rat plasma. Plasma samples were extracted with diethyl ether and separated on an ACQUITY UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) using gradient elution consisting of 0.1% formic acid in water (A) and methanol (B). The multiple reaction monitoring (MRM) mode with electrospray ionization in the positive ion mode was used for detection. The linear range was 0.1 ng/mL to 50 ng/mL for chrysin and tectochrysin, respectively. The accuracy (relative error, RE%) ranged from −8.8% to 7.5% and the intra-day and inter-day precision were within 15% and had a mean extraction recovery rate of 80.3% to 86.7%. The validated method was applied to a comparative pharmacokinetic study after oral administration of Alpinia oxyphylla fruit ethanol extract between normal rats and dementia rats. The area under the curve (AUC) and peak plasma concentration (Cmax) of the two constituents were remarkably increased in dementia rats than in normal rats.

scholarly journals Simultaneous Determination of Bufalin and Its Nine Metabolites in Rat Plasma for Characterization of Metabolic Profiles and Pharmacokinetic Study by LC–MS/MS

Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1662
Author(s):  
Wenlong Wei ◽  
Yang Yu ◽  
Xia Wang ◽  
Linhui Yang ◽  
Hang Zhang ◽  
...  
Keyword(s):  
Oral Administration ◽  
Simultaneous Determination ◽  
Pharmacokinetic Study ◽  
Metabolic Pathways ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Limit Of Quantitation

Characterization and determination of metabolites to monitor metabolic pathways play a paramount role in evaluating the efficacy and safety of medicines. However, the separation and quantification of metabolites are rather difficult due to their limited contents in vivo, especially in the case of Chinese medicine, due to its complexity. In this study, an effective and convenient method was developed to simultaneously quantify bufalin and its nine metabolites (semi-quantitation) in rat plasma after an oral administration of 10 mg/kg to rats. The prototype and metabolites that were identified were subsequently quantified using positive electrospray ionization in multiple reaction monitoring (MRM) mode with transitions of m/z 387.4→369.6 and 387.4→351.3 for bufalin, m/z 513.7→145.3 for IS, and 387.4→369.6, 419.2→365.2, and 403.2→349.2 for the main metabolites (3-epi-bufalin, dihydroxylated bufalin, and hydroxylated bufalin, respectively). The method was validated over the calibration curve range of 1.00–100 ng/mL with a limit of quantitation (LOQ) of 1 ng/mL for bufalin. No obvious matrix effect was observed, and the intra- and inter-day precisions, as well as accuracy, were all within the acceptable criteria in this method. Then, this method was successfully applied in metabolic profiling and a pharmacokinetic study of bufalin after an oral administration of 10 mg/kg to rats. The method of simultaneous determination of bufalin and its nine metabolites in rat plasma could be useful for pharmacokinetic–pharmacodynamic relationship research of bufalin, providing experimental evidence for explaining the occurrence of some adverse effects of Venenum Bufonis and its related preparations.

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