Gengli Duan

In this study, a reliable and rapid method based on ultra high performance liquid chromatography combined with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS) technology and MetabolitePilot^MT software was developed for berberine metabolites identification in rat plasma. The chemical structures of the metabolites and their product ions were tentatively characterized or identified according to the molecular weights detected and MS/MS data. In all, nine metabolites, including M1 (demethyleneberberine, C₁₉H₁₈NO₄, m/z 324), M2 (glucuronic acid-conjugated demethyleneberberine, C₂₅H₂₆NO₁₀, m/z 500), M3 (diglucuronide-conjugated demethyleneberberine, C₃₁H₃₄NO₁₆, m/z 676), M4 (glucuronic acid-conjugated jatrorrhizine or glucuronic acid-conjugated columbamine, C₂₆H₂₈NO₁₀, m/z 514), M5 (berberrubine or thalifendine, C₁₉H₁₆NO₄, m/z 322), M6 (glucuronic acid-conjugated berberrubine or glucuronic acid-conjugated thalifendine, C₂₅H₂₄NO₁₀, m/z 498), M7 (sulfite-conjugated berberrubine or sulfite-conjugated thalifendine, C₁₉H₁₆NO₇S, m/z 402), M8 (dihydroxy berberrubine or dihydroxy thalifendine, C₁₉H₁₆NO₆, m/z 354) and M9 (dihydroxy berberine, C₂₀H₁₈NO₆, m/z 368) were tentatively characterized or identified. Several new deposition patterns and three new metabolites (M7, M8 and M9) are reported in this paper for the first time. This work not only provides significant insights into the understanding of the metabolic pathways of berberine, but also contributes in identifying potential active drug candidates from the metabolites.

Background: Chiral analysis is a crucial way to differentiate selegiline (SG) intake from drug abuse. Oral fluid (OF) has been successfully used as an alternative matrix for blood testing in several pharmacokinetic studies.Objective: The aim of this study is to describe the pharmacokinetics of SG and its main metabolites in OF after a single oral administration of SG which is meaningful for results interpretation in forensic analysis.Methods: Ten milligrams of SG were orally administered to 8 volunteers, and OF samples were collected for up to 96 hours by having participants spit into polypropylene tubes without stimulation. These samples were submitted to liquid–liquid extraction before analysis by liquid chromatography–tandem mass spectrometry operating in positive ion multiple‐reaction monitoring mode.Results and conclusions: After oral administration, each analyte could be detected in OF specimens from all volunteers with an initial detection time of 0.50 hours. The C_max values of SG, R‐MA, R‐AM and DM‐SG were 50.93–992.67 ng/mL, 29.78–653.64 ng/mL, 8.22–150.15 ng/mL, and 4.34–16.25 ng/mL, respectively, at 0.5 hours, 1–11 hours, 1.5–11 hours, and 0.5–6 hours post dose. The times when the compounds were last determined in OF were 5–24 hours for SG, 52–96 hours for R‐MA, 31–96 hours for R‐AM, and 13–31 hours for DM‐SG after oral administration. There is a period of time in OF in which only MA and AM are present without SG and DM‐SG after a single dose of SG. The pharmacokinetic data could provide supplementary interpretation for OF tests in forensic science and drug treatment programs.

Uncaria rhynchophylla is woody climber plant distributed mainly in China and Japan, the stems and hooks of which can be collected as “Gou-Teng” for the treatment of hyperpyrexia, epilepsy and preeclampsia. Fudan University first manufactured KHR98, the extract of Uncaria rhynchophylla. In order to study the active components and structural information of KHR98, we established a HPLC coupled with quadrupole time-of-flight (Q-TOF)-MS method for rapid analysis of alkaloids. In qualitative analysis, a total of eight compounds, including four known alkaloids and four unknown components, were detected and identified. The fragmentation behaviors, such as the fragment ion information and the fragmentation pathways of the eight components were summarized simultaneously, and the concentration of the above components was determined by HPLC-MS method. The quantitative method was proved to be reproducible, precise and accurate. This study shed light on the standardization and quality control of the KHR98 and provided a foundation for the further research on pharmacology, follow-up clinical research and New Drug Applications.

Abstract A new, simple, and fast infrared-assisted self enzymolysis extraction (IRASEE) approach for the extraction of total flavonoid aglycones (TFA) mainly including baicalein, wogonin, and oroxylin A from Scutellariae Radix is presented to enhance extraction yield. Extraction enzymolysis temperature, enzymolysis liquid-to-solid ratio, enzymolysis pH, enzymolysis time and infrared power, the factors affecting IRASEE procedure, were investigated in a newly designed, temperature-controlled infrared-assisted extraction (TC-IRAE) system to acquire the optimum analysis conditions. The results illustrated that IRASEE possessed great advantages in terms of efficiency and time compared with other conventional extraction techniques. Furthermore, the mechanism of IRASEE was preliminarily explored by observing the microscopic change of the samples surface structures, studying the main chemical compositions change of the samples before and after extraction and investigating the kinetics and thermodynamics at three temperature levels during the IRASEE process. These findings revealed that IRASEE can destroy the surface microstructures to accelerate the mass transfer and reduce the activation energy to intensify the chemical process. This integrative study presents a simple, rapid, efficient, and environmental IRASEE method for TFA extraction which has promising prospects for other similar herbal medicines. ᅟ

Discussion about the Quality Standard Teaching of the Pharmacy Undergraduate Students

In this paper, a facile extraction strategy is reported for the analysis of isopentenyl pyrophosphate, a key isoprenoid, based on magnetic core–shell microspheres with Ti⁴⁺ ion exterior walls coupled with liquid chromatography and tandem mass spectrometry. Because of their excellent hydrophilicity and biological compatibility, the polydopamine@Fe₃O₄-Ti⁴⁺ microspheres display ideal IPP extraction efficiency. The technique includes three steps: sample loading, non-phosphate washing and phosphate elution. Moreover, the microspheres can be regenerated by thorough washing with a specific solvent and can be reused multiple times. The liquid chromatography with tandem mass spectrometry separation was performed on a Welch Ultimate® XB-C₁₈ column with a total chromatographic analysis time of 5 min; the analytical recovery was 98.52%. The proposed method was used to determine the isopentenyl pyrophosphate concentration in rat plasma samples collected from the Shanghai Chest Hospital. The results indicate the prospective value of the as-made microspheres for the sensitive and selective enrichment of phosphate compounds in complicated matrices. This article is protected by copyright. All rights reserved