一种用于中药纯化过程的近红外光谱分析新方法

针对中药大孔吸附树脂纯化过程缺乏在线检测分析手段等问题，提出基于光纤 近红外透射光谱的过程分析新方法．以黄连提取物为例，采用HPLC分析测定值作参 比，用偏最小二乘算法建立了近红外透射光谱校正模型，并成功地用于预测黄连生 物碱在大孔树脂纯化过程中的洗脱曲线．本方法实时、快速，可同时测定洗脱物中 盐酸小檗碱、盐酸巴马亭、盐酸药相碱和黄连总生物碱的浓度．预测精度满足工业 过程分析要求，为提高中药质量分析水平提供了新的途径．     

A study for quality evaluation of Taxilli Herba from different hosts based on fingerprint-activity relationship modeling and multivariate statistical analysis

In this study, a fingerprint-activity relationship modeling between chemical fingerprints and antirheumatic activity was established, and multivariate statistical analysis was used to evaluate the quality of Taxilli Herba (TH) from different hosts. Characteristic fingerprints of 20 batches of TH samples were generated by high-performance liquid chromatography coupled with triple quadrupole-time of flight tandem mass spectrometry (HPLC-Triple TOF-MS/MS), and the similarity analysis was calculated based on thirteen common characteristic peaks by hierarchical clustering analysis (HCA). Subsequently, nine efficacy markers were discovered by combining fingerprints and antirheumatic activity through grey correlation analysis (GCA) and bivariate correlation analysis (BCA). Meanwhile, the content of 5 constituents in 9 markers was determined by high-performance liquid chromatography coupled with triple quadrupole-linear ion trap tandem mass spectrometry (HPLC-QTRAP-MS/MS). The comprehensive quality of TH was assessed using multivariate statistical analysis, including principal components analysis (PCA) and technique for order preference by similarity to ideal solution (TOPSIS). The results showed that a high dose of TH extract could markedly ameliorate arthritis damage compared to other doses, with flavonoids playing an important role in the antirheumatic activity. The comprehensive quality of samples from Morus alba L. (SS) was superior to those from Liquidambar formosana Hance (FXS). The present study will demonstrate the markers associated with efficacy, and provide an applicable strategy for more comprehensive quality control and evaluation of TH.     

Computer Handling of Chemical and Biological Data of Traditional Chinese Medicines

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The polyphenolic profiles and antioxidant effects of Agastache rugosa Kuntze (Banga) flower,leaf, stem and root

Agastache rugosa Kuntze (Korean mint) is used as a spice and in folk medicine in East Asia. The present study identified a total of 18 polyphenols from the flower, leaf, stem and roots of this plant using high‐performance liquid chromatography–tandem mass spectrometry. Fourteen of these compounds had not previously been identified in these plant tissues. Each polyphenol was validated in comparison with external calibration curves constructed using structurally related compounds, with determination coefficients >0.9993. The limits of detection and quantification were 0.092–0.650 and 0.307–2.167 mg/L, respectively. Recoveries of 61.92–116.44% were observed at two spiking levels, with 0.91–11% precision, expressed as relative standard deviation (except anthraquinone spiked at 10 mg/L). Hydroxycinnamic acid was the most abundant compound in the root, while the flowers showed the highest total flavonoid level. Antioxidant activities, determined in terms of reducing power, Fe²⁺ chelating activity and the radical scavenging activities using α,α‐diphenyl‐β‐picrylhydrazyl and 2‐2?‐azino‐bis‐3‐ethylbenzothiazoline‐6‐sulfonic acid, increased in a concentration‐dependent manner; the highest activity was identified in the stems, followed by leaves > flowers > roots. These findings indicate that A. rugosa is a good source of bioactive compounds and can be used as a functional food. Copyright © 2015 John Wiley & Sons, Ltd.     

A UPLC‐TOF/MS‐based metabolomics study of rattan stems of Schisandra chinensis effects on Alzheimer's disease rats model

A UPLC‐TOF/MS‐based metabolomics method was established to explore the therapeutic mechanisms of rattan stems of S. chinensis (SCS) in Alzheimer's disease (AD). Experimental AD model was induced by intra‐hippocampal Aβ_1–42 injection in rats. Cognitive function and oxidative stress condition in brain of AD rats were assessed using Morris water maze tests and antioxidant assays [malondialdehyde (MDA), superoxide dismutase (SOD) and glutathione peroxidase (GSH‐Px)], respectively. UPLC‐TOF/MS combined with multivariate statistical analysis were conducted to study the changes in metabolic networks in serum of rats. The results indicated that the AD model was established successfully and the inducement of Aβ_1–42 caused a decline in spatial learning and memory of rats. The injection of Aβ_1–42 in rat brains significantly elevated the level of MDA, and reduced SOD and GSH‐Px activities. In addition, SCS showed significant anti‐AD effects on model rats. A total of 30 metabolites were finally identified as potential biomarkers of AD and 14 of them had a significant recovery compared with the AD model after SCS administration. Changes in AD metabolite profiling were restored to different levels through the regulation of 13 pathways. This is first report on the use of the UPLC‐TOF/MS‐based serum metabolomics method to investigate therapeutic effects of SCS on AD, and enrich potential biomarkers and metabolic networks of AD.     

Ultra high performance liquid chromatography coupled with electrospray ionization/quadrupole time‐of‐flight mass spectrometry for the rapid analysis of constituents in the traditional Chinese medicine formula Wu Ji Bai Feng Pill

An ultra high performance liquid chromatography coupled with electrospray ionization quadrupole time‐of‐flight mass spectrometry method in both positive and negative ion modes was established in order to comprehensively investigate the major constituents in Wu Ji Bai Feng Pill. Briefly, a Waters ACQUITY UPLC HSS C₁₈ column was used to separate the aqueous extract of Wu Ji Bai Feng Pill. A total of 0.1% formic acid in acetonitrile and 0.1% aqueous formic acid v/v were used as the mobile phase. All analytes were determined using quadrupole time‐of‐flight mass spectrometry with electrospray ionization source in positive and negative ion modes. At length, a total of 173 components including flavones and their glycosides, monoterpene glycosides, triterpene saponins, phenethylalchohol glycosides, iridoid glycosides, phthalides, tanshinones, phenolic acids, sesquiterpenoids and cyclopeptides were identified or tentatively characterized in Wu Ji Bai Feng Pill in an analysis of 16.0 min based on the accurate mass and tandem mass spectrometry behaviors. The developed method is rapid and highly sensitive to characterize the chemical constituents of Wu Ji Bai Feng Pill, which could not only be used for chemical standardization and quality control of Wu Ji Bai Feng Pill, but also be helpful for further study in vivo metabolism of Wu Ji Bai Feng Pill.     

Metabonomic analysis of serum reveals antifatigue effects of Yi Guan Jian on fatigue mice using gas chromatography coupled to mass spectrometry

Yi Guan Jian (YGJ), one of the most commonly used traditional Chinese medicines, has been reported to possess significant antifatigue effects. However, the mechanisms underlying its antifatigue effects remain largely unresolved. In this study, a metabonomics approach, involving gas chromatography coupled to mass spectrometry and a multivariate statistical technique, was developed to estimate the extent to which YGJ alleviated the exhausting swimming‐induced fatigue of mice. High‐dose treatment with YGJ significantly extended the swimming time of fatigued mice. Significant alterations of metabolites involving amino acids, organic acids and carbohydrates were observed in the serum of fatigued mice, which were reversed by YGJ treatment while biochemical indexes returned to normal. These metabolic changes suggest that the antifatigue effect of YGJ is associated with the impairement of amino acid, organic acids and carbohydrates. It also appears that YGJ can induce significant metabolic alterations independent of the exhausting swimming‐induced metabolic changes. The significantly altered metabolites induced by YGJ intervention include l‐ 2‐amino‐acetoacetate, taurine, fumaric acid, malic acid, oxoadipic acid and l‐ aspartate, all of which are associated with antifatigue properties. This suggests that YGJ exerts chemopreventive effects via antifatigue mechanisms.     

Coordination Complexes to Combat Bacterial Infections: Recent Developments,Current Directions and Future Opportunities

Drug discovery aimed at the efficient eradication of life-threatening bacterial infections, especially in light of the emergence of multi-drug resistance of pathogenic bacteria, has remained a challenge for medicinal chemists over the past several decades. As nutrient acquisition and metabolism at the host-pathogen interface become better elucidated, new drug targets continue to emerge. Metal homeostasis is among these processes, and thus provides opportunities for medicinal inorganic chemists to alter or disrupt these processes selectively to impart bacteriostatic or bacteriotoxic effects. In this minireview, we showcase some of the recent work from the field of metal-based antibacterial agents and highlight divergent strategies and mechanisms of action.     

Simultaneous determination of eight Danshen polyphenols in rat plasma and its application to a comparative pharmacokinetic study of DanHong injection and Danshen injection

Polyphenols derived from Danshen are responsible for the therapeutic effects of DanHong injection, a two‐herb combination of Danshen and Honghua. Whether the pharmacokinetics of Danshen polyphenols is changed by coexisting Honghua constituents remains unknown. A sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed in this study for simultaneous determination of eight Danshen polyphenols (i.e., protocatechuic aldehyde, protocatechuic acid, tanshinol, salvianolic acid D, rosmarinic acid, salvianolic acid A, lithospermic acid, and salvianolic acid B) in rat plasma and applied to a comparative pharmacokinetic study of DanHong injection and Danshen injection. Liquid chromatography conditions, mass spectrometry parameters, and sample preparation were optimized step by step. The calibration curves showed good linearity (r > 0.99) for all the polyphenols. The mean extraction efficiencies ranged from 62.2 to 88.7% with negligible matrix effects. The intrabatch and interbatch precision at all the quality control levels were less than 15% of the nominal concentrations with accuracy of 88.8–114%, except that precision and accuracy at lower limit of quantitation were 3.2–17.3 and 95.7–119%, respectively. Comparative pharmacokinetic study suggested that the coexisting Honghua constituents might have negligible influences on the pharmacokinetics of Danshen polyphenols from DanHong injection. The bioanalytical method could also be applied to pharmacokinetic studies of other Danshen herbal products.