ABSTRACT
A rapid and sensitive ultra fast liquid chromatography tandem mass spectrometry method (UFLC-MS/MS) was developed and validated for the simultaneous determination of six Saikosaponins (SSs) (SSa, SSb1, SSb2, SSd, SSc, SSf) of Bupleurum Dropping Pills (BDP) in rat plasma using chloramphenicol as the internal standard (IS). The SSs were separated using an ACQUITY UPLC(®) BEH C18 column (50 mm × 2.1mm, 1.7 µm) and detection of these compounds were done by using a Qtrap 5500 mass spectrometer coupled with negative electrospray ionization (ESI) source under the multiple reaction monitoring (MRM) mode. According to regulatory guidelines, the established method was fully validated and results were showed within acceptable limits. The lower limit of quantifications (LLOQs) of all analytes were 0.2 ng/mL. The validated method was successfully applied into a pharmacokinetic study of orally administered BDP in rats.
Subject(s)
Bupleurum/chemistry , Oleanolic Acid/analogs & derivatives , Plant Extracts/administration & dosage , Saponins/pharmacokinetics , Administration, Oral , Animals , Limit of Detection , Oleanolic Acid/blood , Oleanolic Acid/pharmacokinetics , Rats , Reference Standards , Saponins/blood , Spectrometry, Mass, Electrospray Ionization , Tandem Mass SpectrometryABSTRACT
A simple, rapid and sensitive liquid chromatography with tandem mass spectrometry (LC-MS/MS) method for the determination of periplocymarin in biological samples was developed and successfully applied to the pharmacokinetic and tissue distribution study of periplocymarin after oral administration of periplocin. Biological samples were processed with ethyl acetate by liquid-liquid extraction, and diazepam was used as the internal standard. Periplocymarin was analyzed on a C18 column with isocratic eluted mobile phase composed of methanol and water (containing 0.1% formic acid) at a flow rate of 0.2 mL/min (73:27, v/v). Detection was performed on a triple-quadrupole tandem mass spectrometer using positive-ion mode electrospray ionization in the selected reaction monitoring mode. The MS/MS ion transitions monitored were m/z 535.3â355.1 and 285.1â193.0 for periplocymarin and diazepam, respectively. Good linearity was observed over the concentration ranges. The lower limit of quantification was 0.5 ng/mL in plasma and tested tissues. The intra-and inter-day precisions (relative standard deviation) were <10.2 and 10.5%, respectively, and accuracies (relative error) were between -6.8 and 8.9%. Recoveries in plasma and tissue were >90%. The validated method was successfully applied to the pharmacokinetic and tissue distribution studies of periplocymarin in rats. Copyright © 2016 John Wiley & Sons, Ltd.
