Identification and determination of the major constituents in Kai‐Xin‐San by UPLC‐Q/TOF MS and UFLC‐MS/MS method

Abstract

In order to have overall chemical material information of Kai-Xin-San (KXS), the reliable ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometer (UHPLC-Q-TOF-MS) and ultra-fast liquid chromatography mass spectrometer (UFLC-MS/MS) methods were developed for the identification and determination of the major constituents in KXS. Moreover, the UHPLC-Q-TOF-MS method was also applied to screen for multiple absorbed components in rat plasma after oral administration of KXS. The UHPLC-Q-TOF-MS method was achieved on Agilent 6520 Q-TOF mass and operated in the negative ion mode. Good separation was performed on a ZORBAX Eclipse Plus C18 column with a gradient elution at a flow rate of 0.2 ml/min. A total of 92 compounds in KXS were identified or tentatively characterized based on their exact molecular weights, fragmentation patterns, and literature data. A total of 26 compounds including 23 prototype components and three metabolites were identified in rat plasma after oral administration of KXS. Then, 16 major bioactive constituents were chosen as the benchmark substances to evaluate the quality of KXS. Their quantitative analyses were performed by a triple quadrupole tandem mass spectrometer (MS/MS) operating in multiple-reaction monitoring mode(MRM). The analysis was completed with a gradient elution at a flow rate of 0.4 ml/min within 35 min. The simple and fast method was validated and showed good linearity, precision, and recovery. Furthermore, the method was successful applied for the determination of 16 compounds in KXS. All results would provide essential data for identification and quality control of active chemical constituents in KXS. Copyright © 2016 John Wiley & Sons, Ltd.

Phytochemical Analysis and Total Antioxidant Capacity of Rhizome, Above‐Ground Vegetative Parts and Flower of Three Iris Species

“…[30] Compound 7 at 6.23 min and 567 m/z was tentatively marked as polygalaxanthone III, according to available literature about chemical constituents in Kai-Xin-San herb formula. [31] The last one from the xanthones group, bellidifolin (273 m/z; compound 11), previously isolated from rhizomes of I. nigricans, [32] was found in the current study in I. pumila rhizome and above-ground vegetative parts ( Table 1). It produced MS 2 base peak at 258 m/z (corresponding to loss of methyl group) and MS 3 base peak at 230 m/z (formed by further loss of CO group).…”

Solvent-Free Synthesis of High-Purity Sucrose Fatty Acid Monoesters and a Comparison of Their Properties with Those of Their Commercial Counterparts

“…While these methods can effectively quantify SE content, they are time-consuming and require high concentrations of analytes. In recent years, UPC 2 -MS has emerged as a highly effective tool for the accurate quantitation of various components in complex mixtures − and was thus used in the study presented here…”

A practical method for rapid discrimination of constituents in Psoraleae Fructus by UPLC‐Q‐Orbitrap MS

“…Traditional Chinese medicine (TCM) is a group of complex mixtures consisted of different chemical components. Due to it having extensive effects via multiple components, multiple pathways, and multiple targets, as well as its special benefits of low toxicity but positive effectiveness, less susceptibility to drug resistance, and dual‐directional regulation, TCM has gained increasing attention both domestically and internationally 1–3 . However, its complicated chemical composition has made the substances and mechanism investigate of pharmacodynamics become a thorny point in the way of TCM towards modernization and hinders quality control, safety evaluation, and further development, as well as its utilization.…”