Rapid characterization of the constituents in Jigucao capsule using ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry

Jigucao capsule is a well-known Chinese patent medicine for the treatment of acute and chronic hepatitis and cholecystitis. The chemical components of Jigucao capsule were not clear resulting from the paucity of relevant studies, which hindered the research of the pharmacological mechanism, the comprehensive development, and utilization of Jigucao capsule in clinical studies. By establishing a high-throughput ultra-performance liquid chromatography quadrupole time of flight mass spectrometry in combination with intelligent UNIFI software data processing platform to automatically characterize and identify the chemical profile of Jigucao capsule, 144 compounds were determined rapidly, including 34 terpenoids, 25 flavonoids, 22 steroids, 21 phenylpropanoids, 10 glycosides, six alkaloids, 13 organic acids, and other 13 components. These compounds may be the active components of Jigucao capsule. In this study, a rapid and robust method for comprehensively analyzing the chemical composition of Jigucao capsule was described and established for the first time. The results will provide a reference for the quality control of Jigucao capsule and the establishment of a higher quality standard, as well as for the pharmacodynamic material basis research.     

Chemical profiling and quantification of multiple components in Jin-Gu-Lian capsule using a multivariate data processing approach based on UHPLC-Orbitrap Exploris 240 MS and UHPLC-MS/MS

The Jin-Gu-Lian capsule, a Chinese Miao herbal compound, is widely used to treat rheumatoid arthritis. In this study, a rapid, selective, and sensitive UHPLC-Orbitrap Exploris 240 MS method was developed to analyze the chemical composition of Jin-Gu-Lian capsules. A total of 88 compounds were identified, including 23 flavonoids, 23 organic acids, 14 phenylpropanoids, 12 phenols, eight alkaloids, four terpenes, three quinones, and one ketone. Among these, 21 compounds were clearly detected based on a comparison with reference standards and selected as quality control markers. Thereafter, these compounds were simultaneously determined in the Jin-Gu-Lian capsules. The established method was successfully validated and applied for the simultaneous determination of 21 biologically active compounds in Jin-Gu-Lian capsules of 27 sample batches. Quantitative data of the analytes were analyzed using multivariate statistical analysis to determine the quality of the Jin-Gu-Lian capsules. Four compounds (JGLC6 [salidroside], JGLC8 [chlorogenic acid], JGLC12 [liriodendrin], JGLC19 [quercetin]) were identified as chemical markers for quality control of Jin-Gu-Lian capsules. Altogether, the established method was validated as a novel and efficient tool, that can be used for rapid analysis of Jin-Gu-Lian capsules. Accordingly, this study serves as a reference for scientific research on traditional Chinese and ethnic medicine.     

球形黑腔辐射输运问题的蒙特卡罗模拟

利用蒙特卡罗方法模拟六孔球形黑腔中的辐射输运, 研究靶球辐照均匀性问题. 对于几何结构简单的解析模型, 研究了不同黑腔靶球半径比的靶球辐照均匀性变化规律, 得出的结论与解析的“视因子”方法给出的一致. 对于几何结构复杂的黑腔模型, 如放置有挡板的模型, 解析方法计算困难, 但利用蒙特卡罗方法仍然能够准确模拟计算. 不同挡板大小的理论模型计算结果表明, 挡板对X光输运到靶球表面的分布状况有明显的影响, 如果设置得当则可以提高X光利用效率并显著改善靶球辐照均匀性, 否则可能严重破坏靶球辐照均匀性. 因此, 黑腔中的挡板位置及大小需要精心设计. 应用表明, 蒙特卡罗方法对于具有复杂结构的黑腔辐射输运问题具有很好的适应性.     

火焰原子吸收光谱法分析竹沥胶囊中铁、锌、锰的含量

用火焰原子吸收光谱法测定了竹沥胶囊中铁、锌、锰3种微量元素含量,结果表明,竹沥胶囊中铁为57.8μg/g,锌为16.5μg/g,锰为8.13μg/g,各元素回收率在98%～107%之间。     

The Analysis of Theophylline — Containing Pharmaceuticals by Room Temperature Phosphorescence

Abstract

A simple and specific technique is used in analyzing pharmaceutical preparations (capsules, elixirs, syrups, and tablets) for theophylline and related compounds. The procedure consists of dissolving (diluting) appropriate amounts of the preparations and standards in (with) a 1 M KI-water solution, spotting 5 μL of each resultant solution onto filter paper discs, determining the phosphorescence intensities at room temperature and comparing sample signal levels to those of standards. The quantities of active ingredients and standards used in the determinations ranged from 25 ng to 1 μg. The results indicate that room temperature phosphorescence is useful for analyzing pharmaceutical preparations where active ingredients are usually contained in a wide variety of matrices.     

Recognition of Multiple Methyl Groups on Aromatic Rings by a Polyaromatic Cavity

The methyl group is a small substituent, usually showing relatively weak or no interactions with other functional groups and metal ions. Herein, we present the recognition of the number of methyl groups on synthetic and natural aromatic compounds (i.e., benzene and xanthine derivatives, respectively) by the 1 nm‐sized polyaromatic cavity of a coordination capsule in water. Detailed competitive encapsulation experiments as well as X‐ray crystallographic analysis revealed that multiple guest–host CH₃–polyaromatic interactions in the confined nanospace are key driving forces for the high selectivity.     

Dynamic Equilibrium between a Supramolecular Capsule and Bowl Generated by Inter‐ and Intramolecular Metal Clipping

The metal‐induced self‐assembly of a resorcin[4]arene derivative 1 that has four pyridine units as pendent groups and two equivalents of [M(dppp)(OTf)₂] (M=Pd, Pt) results in a dynamic equilibrium between an interclipped supramolecular capsule 3 and an intraclipped bowl 4 in nitromethane, although the interclipped capsule 3 is formed as a sole adduct in chloroform/methanol and the intraclipped bowl 4 is formed exclusively in an aqueous phase. This demonstrates how metal‐induced self‐assembly can be tuned by subtle changes in the solvent system. The coexistence of the two structures in nitromethane was characterized by NMR spectroscopy and coldspray ionization mass spectrometry (CSI‐MS). The crystal structure of the interclipped capsule 3 b , which is composed of two units of ligand 1 and four Pt^II ions, reveals the capsule cavity to have nanoscale dimensions of 15×20 Å. NMR spectra show that the dynamic equilibrium between 3 and 4 is dependent on concentration and temperature. Temperature‐dependent ¹H NMR spectroscopy was carried out from 273 to 343 K to verify the thermodynamic parameters that control the dynamic equilibrium process; the conversion from the interclipped supramolecular capsule 3 a to the intraclipped bowl 4 a is entropically favored and enthalpically disfavored. The rotational barrier of the restricted rotation of pyridine units in the intraclipped bowl 4 was determined by line‐shape analysis.     

含浸P204胶囊的芯材缓释与功能性研究

对于含浸10个碳以上双链型表面活性剂的微胶囊体系,已得到了受温度、电场、pH值、化学反应及光控制的功能性胶囊~[1～3].功能性胶囊对芯材的缓释及控制释放作用,在医药、生化等方面的应用具有广阔的前景.但是一般认为对于含浸的双键型表面活性剂的较短链链长不能小于10个碳,对含浸链长小于10个碳的表面活性剂的功能性微胶囊体系未见报道.     

A hexagonal columnar packing structure of C7 symmetric supramolecules: a superstructure of a 2:3 complex of heptakis‐(6‐O‐tert‐butyldimethylsilyl)‐β‐cyclodextrin and ethyl acetate

The recrystallization of Heptakis[6‐O‐tert ‐butyldimethylsilyl)]‐β ‐cyclodextrin ( 1 ) from ethyl acetate gave single crystals of 1 ₂·(ethyl acetate)₃ complex. The superstructure of 1₂·(ethyl acetate)₃ complex was investigated by ¹H NMR spectroscopy, molecular modeling, and single crystal/powder X‐ray diffractions. Encapsulation of ethyl acetate molecules with 1 and a unique hexagonal columnar superstructure in its crystal were found. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)