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A selective and sensitive ultra‐high‐performance liquid chromatography‐tandem mass spectrometry method was developed and validated for the determination of three triterpenoid saponins isolated from Astragalus membranaceus leaf extract. In this article, a method for simultaneous determination of Huangqiyenin A, Huangqiyenin E, and Huangqiyenin K was established for the first time. The method was successfully applied to the pharmacokinetic study of Astragalus membranaceus leaf extract after oral administration. Liquid–liquid extraction was applied to plasma sample preparation. Multiple reaction monitoring mode with an electrospray ion source in positive electrospray ionization was chosen to quantify the analytes. Chromatographic separation was performed on a Waters HSS T3 column, using gradient elution with a mobile phase composed of acetonitrile and 5 mM ammonium acetate/water. The pharmacokinetic results showed that all three compounds had the characteristics of rapid absorption‐slow metabolism trend. The time of maximum plasma concentration of Huangqiyenin A is higher than Huangqiyenin E and Huangqiyenin K. And the maximum plasma concentration of Huangqiyenin A is higher as well. The pharmacokinetic results revealed the pharmacokinetic characteristics of the three analytes in rat plasma, which could provide a helpful reference for the further study of Astragalus membranaceus leaf extract. [ABSTRACT FROM AUTHOR]

Objective: A sensitive and rapid ultra‐high‐performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was successfully applied to the determination of 10 alkaloids in beagle dog plasma following a single oral dose of Xiatianwu capsules and enteric‐coated capsules, with theophylline serving as the internal standard (IS). Methods: Plasma samples were preprocessed using liquid–liquid extraction (LLE) with ethyl acetate ahead to separation using a gradient elution procedure on a Waters ACQUITY UPLC HSS T3 column (1.8 μm, 100 × 2.1 mm). The mobile phase was composed of 0.1% formic acid solution and acetonitrile at the flow rate of 0.3 ml/min. Multiple reaction monitoring (MRM) was used to determine the analytes in the positive ion mode. Results: The calibration curves for 10 analytes demonstrated a high degree of linearity (r ≥ 0.9920). The lower limit of quantification (LLOQ) values for 10 alkaloids were all more than 1.074 ng/ml, and matrix effects varied from 94.25% to 106.15%. The mean extraction recovery of quality control samples at low (LQC), medium (MQC) and high (HQC) concentrations, as well as IS, was all more than 76.60%. The intra‐day and inter‐day precision (RSD) also satisfied the requirement. Simultaneously, the variation of assay accuracies (RE) was between 13.05% and 9.38%. Conclusion: The test was validated in accordance with regulatory bioanalytical guidelines and was found to be suitable for use in a pharmacokinetic investigation of these compounds in beagle dogs after oral administration of Xiatianwu general capsules and enteric‐coated capsules. The Cmax of 10 alkaloids ranged from 52.61 to 192.46 ng/ml after oral administration of Xiatianwu capsules, and from 67.50 to 247.36 ng/ml. The Tmax was between 0.59 and 1.33 h of Xiatianwu capsules, and between 1.08 and 2.00 h of enteric‐coated capsules. The t1/2 ranged from 3.18 to 7.47 h of general capsules, and from 6.01 to 11.36 h. AUC0‐t ranged from 181.06 to 722.74 ng·h/ml of Xiatianwu capsules, and from 275.03 to 884.17 ng·h/ml of enteric‐coated capsules. The Cmax of enteric‐coated capsules were significantly increased except for tetrahydropalmatine and berberine. Tmax of general capsules were less than 1 h, and of enteric‐coated capsules were less than 2 h. The t1/2 of dehydrocorydaline, palmatine, tetrahydrojatrorrhizine, jatrorrhizine and coptisine in enteric‐coated capsules was longer than that in ordinary capsule. The AUC0‐t and AUC0‐∞ of bicuculline, dehydrocorydaline, protopine, magnoflorine, tetrahydrojatrorrhizine, jatrorrhizine, berberine and coptisine were all significantly higher in enteric‐coated capsules. [ABSTRACT FROM AUTHOR]

A specific, simple, and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method utilizing the Triple Quad system has been developed and validated for the simultaneous determination and pharmacokinetic study of four triterpenoid components of Acanthopanax sessiliflorus in rat plasma. The components are 22-α-hydroxychiisanogenin, chiisanogenin, (1R,11α)1,4-epoxy-11-hrdroxy-3,4-secolupane-20(30)-ene-3,28-dioic acid, and 22-α-hydroxychiisanoside. Sample preparation involved a liquid-liquid extraction of the analytes with ethyl acetate. Chromatographic separation was accomplished using an Agilent SB-C18 column (1.8 μm, 2.1 mm × 50 mm) with 2.0 min isocratic elution. The compounds were detected with a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode and an ESI source in negative mode. The method was linear for all analytes over the investigated range, with all determined correlation coefficients exceeding 0.9906. The limit of quantification of each analyte was lower than 1 ng/mL. The intraday and interday precisions were less than 14.9%, and the accuracy ranged from -10.2 to 11.8%. The mean recoveries of the analytes were higher than 80.0%, and the matrix effects were between 100.4 and 107.1%. These results may contribute to determining the mechanism of action and guiding the clinical application of Acanthopanax sessiliflorus. [ABSTRACT FROM AUTHOR]

Sanguisorba officinalis L. possesses detoxifying, analgesic, and hemostatic properties. After charred processing, S. officinalis exhibits significantly enhanced medicinal effects. Currently, most pharmacokinetic studies focus on the chemical constituents of unprocessed S. officinalis. There is limited research on the comparison of chemical constituents before and after processing. This study established a pharmacokinetic method using ultra‐high‐performance liquid chromatography‐tandem mass spectroscopy (UHPLC‐MS/MS) to simultaneously determine the levels of four tannin compounds in rat plasma. In negative ion mode, MS/MS detection was performed using an electrospray ionization source. Chromatographic separation was performed using WATERS ACQUITY HSS T3 column (2.1 × 100 mm, 1.8 µm) with a gradient elution of water and acetonitrile as the mobile phase. The pharmacokinetic results indicate that all four compounds reached peak concentrations within 2 h, demonstrating rapid absorption into the bloodstream within the gastrointestinal tract. Notably, the absorption was generally faster in the charred compound of S. officinalis after processing. These four compounds exhibited slower elimination in rat plasma, while in S. officinalis charcoal, the compounds were eliminated more rapidly. The pharmacokinetic results have revealed the pharmacokinetic characteristics of the four analytes in rat plasma which provides valuable reference information for further investigating the in vivo absorption process of S. officinalis after processing. [ABSTRACT FROM AUTHOR]