Simultaneous quantitation of the diastereoisomers of scholarisine and 19‐epischolarisine, vallesamine, and picrinine in rat plasma by supercritical fluid chromatography with tandem mass spectrometry and its application to a pharmacokinetic study

Abstract

Dengtaiye tablet has been used to treat chronic bronchitis cough. Scholarisine, 19-epischolarisine, vallesamine, and picrinine are the representative constituents of Dengtaiye. A rapid and sensitive assay based on supercritical fluid chromatography with tandem mass spectrometry has been developed and validated for the determination of the diastereoisomers of scholarisine and 19-epischolarisine, vallesamine, and picrinine in rat plasma using lamotrigine as internal standard. The analysis in a run time of only 6 min was performed on an ACQUITY UPC(2) Trefoil(TM) BEH 2-EP column (3.0 × 150 mm, 2.5 μm) at 50ºC. The mobile phase consisting of carbon dioxide and methanol (2 mM ammonium formate) was performed as follows: 15% methanol (2 mM ammonium formate) maintained at 0-2 min, 15-19% methanol (2 mM ammonium formate) at 2-4 min, 19-15% methanol (2 mM ammonium formate) at 4-6 min. The flow rate was 1.50 mL/min. The assay was linear over the concentration ranges 50-10000 pg/mL for scholarisine, 19-epischolarisine, vallesamine, and picrinine with corresponding lower limits of quantitation of 50 pg/mL. Intra- and interday precisions were in the range 1.42-12.85% with accuracies in the range -11.71-2.48%. The method was successfully applied to a pharmacokinetic study involving a single oral administration of 108 mg/kg Dengtaiye tablet to rats.

Supercritical Fluid Chromatography in Natural Product Analysis – An Update

“…Although commercial formulations (Dengtaiye tablets, DTY) are available, their pharmacokinetic profile is still poorly explored and in vivo studies are missing. Recently, Yang et al [67] developed a SFC/MS-MS method for the simultaneous quantitation of these four compounds in rat plasma using an Acquity UP-C 2 BEH 2-EP column with 2 mmol ammonium formate in methanol as modifier. The method was subsequently validated (LOQs 50 pg/mL, recoveries between 84.47 and 95.22 %, precision in the range from 1.42 to 12.85 %) and applied to a pharmacokinetic study in rats after oral administration of 108 mg/kg Dengtaiye tablets.…”

Theory and Practice of UHPLC and UHPLC–MS

“…Because SFCeMS is quite a new approach in bioanalysis, many studies focus on detailed optimization of the individual parameters of SFCeMS, including ion source set-up, mobile phase composition, make-up solvent composition, temperature, and BPR pressure (Jumaah et al, 2016;Pilarová et al, 2016;Sen et al, 2016;Yuan et al, 2016;Yang et al, 2016;Spaggiari et al, 2014). Matrix effects are an important obstacle of HPLCeMS and their determination is now obligatory in bioanalytical methods.…”

Pharmacokinetics of the Rac/Cdc42 Inhibitor MBQ-167 in Mice by Supercritical Fluid Chromatography–Tandem Mass Spectrometry

“…These advantages have rendered SFC-coupled MS/MS as a rapid and sensitive analytical method for pharmacokinetic applications. 14−16…”