Simultaneous Determination of Ten Constituents in Chaiqin Qingning Capsule by High-performance Liquid Chromatography Coupled with Triple-quadrupole Mass Spectrometry.

BACKGROUND: Chaiqin Qingning Capsule (CQQNC) was a prescription of Traditional Chinese Medicine with the effects of clearing away heat and removing toxin, harmonizing the exterior and interior, it was widely used in Asian, for example, China and Japan, different batches of the raws materials and different processing time may be the vital factor which raised a challenge to control the quality of the CQQNC. EXPERIMENTAL METHODS: In this experiment, a high-performance liquid chromatography-mass spectrometry/MS (HPLC-MS/MS) method was developed to simultaneously determine ten bioactive components for the quality control of CQQNC. Chromatographic separation was achieved using an XBridge BEH C18 column (150 mm × 4.6 mm, 2.5 µm) with a mobile phase composed of 10 mm aqueous ammonium acetate and acetonitrile using a gradient elution in 20 min. This study was conducted by multiple reaction monitoring mode through electrospray ionization resource with a negative ionization mode. RESULTS: The established method was validated with good performance of precision, accuracy, stability, and reproducibility and was utilized to simultaneously quantify ten constituents of CQQNC obtained from seven different batches. CONCLUSION: It is the first time to report the rapid and simultaneous analysis of the ten compounds in CQQNC by HPLC-MS/MS and apply to determine 10 constituents in 7 batches of CQQNC bought from drug store in china. This method could be considered as good quality criteria to control the quality of CQQNC. SUMMARY: In this paper, a simple, specific, and rapid high-performance liquid chromatogram coupled with triple-quadrupole mass spectrometry method for simultaneous quantification of ten constituents in Chaiqin Qingning Capsule has been developed for the first time. This method could be considered as good quality criteria to control the quality of CQQNC. Abbreviations used: CHM: Chinese herbal medicine; TCM: Traditional Chinese Medicine; CQQNC: Triple-quadrupole mass spectrometry Chaiqin Qingning Capsules; HPLC-MS/MS: High liquid chromatography equipped with tandem mass spectrometry; ESI: Electrospray ionization; DP: Declustering potential; CE: Collision energy; RSD: Relative standard deviation; LOD: Limit of detection; LOQ: Limit of quantity.

Comparative pharmacokinetic study of baicalin and its metabolites after oral administration of baicalin and Chaiqin Qingning capsule in normal and febrile rats.

An accurate, precise, selective, and sensitive high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of baicalin and its metabolite, baicalein 6-O-glucopyranuronoside, in normal and febrile rats plasma. Two analytes, along with hesperidin as an internal standard, were determined by multiple reactions monitoring (MRM) operated in the positive electrospray ionization (ESI) mode. Chromatographic separation was performed on an Agilent ZORBAX Extend-C18 column (100mm×2.10mm, 3.5µm) with a mobile phase of 0.1% formic acid solution and acetonitrile at a flow rate of 0.6mL/min. The calibration curves showed good linearity (r≥0.9974) with the concentration ranges of 2.000-2000ngmL-1 for baicalin and baicalein 6-O-glucopyranuronoside. The inter- and intra-day accuracies (relative error, RE%) were between -6.62% and 6.75%, and the precisions (relative standard deviation, RSD%) were less than 9.09% for quality control samples (QCs). The method also possessed good selectivity, recovery and stability, and was successfully applied to a comparative pharmacokinetic study of baicalin and baicalein 6-O-glucopyranuronoside in normal and febrile rats after oral administration of baicalin and Chaiqin Qingning capsule.

HPLC-Q-TOF-MS/MS Analysis of the Constituents in the Rat Biological Fluids After Oral Administration of Qing Ru Xiao granules.

A high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry method was established to detect as many constituents in rat biological fluids as possible after oral administration of Qing Ru Xiao granules (QRX). An Agilent Poroshell 120 EC-C18 column was adopted to separate the sample constituents, and mass spectra were acquired in positive and negative ion modes. First, the fingerprints of QRX were established, resulting in 28 components being detected within 30 min. Among these compounds, 11 were tentatively identified by comparing the retention times and mass spectral data with those of reference standards and the reference literature; the other 17 components were tentatively assigned solely based on the mass spectrometry data. Furthermore, metabolites in rat plasma and urine after oral administration of QRX were also analyzed. A total of 15 compounds were identified, including 13 prototypes and 2 metabolites through metabolic pathways of oxidation. This is the first systematic study on the metabolic profiling of QRX.

Caesalminaxins A-L, cassane diterpenoids from the seeds of Caesalpinia minax.

Fourteen new cassane diterpenoids, caesalminaxins A-L (1-14), and three known compounds were isolated from the seeds of Caesalpinia minax. Among the new diterpenoids, compounds 3 and 4 possess a rare spiro C/D ring system. The C-16 epimeric mixture 1/2 has an unprecedented carbon skeleton, presumably derived from 3 by cleavage of the C-13-C-14 bond. Compound 5 is the first example of a cassane diterpenoid with a spiro A/B ring system. The structures of the compounds were elucidated on the basis of 1D and 2D NMR analysis, and the absolute configurations of 3, 4, 9, and 11 were determined by single-crystal X-ray crystallography. Biosynthesis pathways for 1/2, 3, and 5 are postulated. Compounds 4, 8, and the known bonducellpin D exhibited moderate activity against four tested human cancer cell lines, HepG-2, K562, HeLa, and Du145.

Guanidine alkaloids from Plumbago zeylanica.

Eleven new guanidine alkaloids, plumbagines A-G (2-8) and plumbagosides A-D (9-12), as well as two known analogues (1, 13), were isolated from the aerial parts of Plumbago zeylanica. Their structures were elucidated by spectroscopic analyses including 1D and 2D NMR, MS, IR, and CD methods. The absolute configuration of 1 was determined by single-crystal X-ray diffraction of its derivative (1a).