Qualitative and quantitative analysis of iridoid glycosides in the flower buds of Lonicera species by capillary high performance liquid chromatography coupled with mass spectrometric detector

A highly sensitive and specific method, based on capillary high performances liquid chromatography coupled with single quadrupole mass spectrometry using electrospray ionization (capillary HPLC-ESI/MS), is proposed for the identification and quantification of iridoid glycosides in the flower buds of five Lonicera species. A Zorbax SB-C18 (0.3 mm × 150 mm, 5 μm) capillary column and a gradient elution with methanol-acetonitrile-aqueous acetate acid were utilized. The most intensive electrospray ionisation signals were found in the negative ion spectra owing to CH₃COO⁻ adducts. Eight iridoid glycosides derived from the flower buds of Lonicera species were analyzed by mass spectrometry: sweroside (IG1), 7-O-ethyl sweroside (IG2), 7-epi vogeloside (IG3), secoxyloganin (IG4), secoxyloganin 7-butyl ester (IG5), dimethyl-secologanoside (IG6), centauroside (IG7), and loganin (IG8) using combined information on retention time, the molecular ion mass and fragment ion masses. Detection limits were lower than 1.9 ng/mL in selected ion monitoring (SIM) mode and all calibration curves showed good linear regression (r² > 0.9938) within test ranges. The validated method was successfully applied to analyze eight iridoid glycosides in the flower buds of five Lonicera species and provided a new basis of assessment on quality of Flos Lonicerae.     

包结物晶析法选择分离辛夷挥发油中1,8-桉叶素

主客体化学的分子识别在同分异构体选择分离、外消旋异构体光学拆分中已有广泛研究[1～3].我们利用中草药挥发油中化学组分的分子形状、几何拓扑性质、官能团数量和键力性质的不同,选定主体分子对挥发油中某一组分进行分子识别,并以结晶的形式从挥发油体系中离析出来,达到选择分离单一挥发油化学组分的目的[4～7].本文利用主体分子1,1,6,6-四苯基-2,4-己二炔-1,6-二醇(A)作为主体分子[8],以辛夷挥发油为研究对象,其主要成分1,8-桉叶素(B)为分子识别的客体分子,与化合物A形成稳定的包结物晶体(A+B),并从辛夷挥发油中析出,得到纯度为100%的…     

Studies on chemical constituents of Flos Puerariae-Semen Hoveniae medicine pair by HPLC and Fourier transform ion cyclotron resonance mass spectrometry

Alcoholic liver disease is currently the most clinically concerning liver disease, which occurs from chronic alcohol abuse. Flos Puerariae and Semen Hoveniae have been used to treat alcohol drinking excessively for thousands of years in China. In this study, the ethanol extract of the medicine pair was qualitatively and quantitatively analyzed by high-performance liquid chromatography and Fourier transform ion cyclotron resonance mass spectrometry. First, the high-performance liquid chromatography fingerprint was established to obtain the overall chromatographic data of its chemical constituents. Next, high-performance liquid chromatography-mass spectrometry was applied to identify its chemical constituents. Then, the characteristic constituents were simultaneously quantified by high-performance liquid chromatography. In addition, the chemical constituents that were absorbed into rat plasma were identified by high-performance liquid chromatography-mass spectrometry. As a result, a total of 48 chemical constituents in the medicine pair were detected and identified in vitro. Meanwhile, the content of seven representative constituents, including dihydromyricetin, glycitin, genistin, tectoridin, glycitein, genistein, and tectorigenin were simultaneously determined. Furthermore, a total of 19 chemical constituents were detected in rat plasma after oral administration. In short, the chemical constituents of the medicine pair were initially investigated in this study, which will lay the foundation for the discovery of its pharmacodynamic substances in further works.     

闹羊花与野菊花红外光谱的分析与鉴定

采用傅里叶变换红外光谱对杜鹃花科植物闹羊花与菊科植物野菊花两种花类中药材的主成分进行表征,其中闹羊花出现在1 648和1 543cm-1出现明显的酰胺Ⅰ带和酰胺Ⅱ带吸收峰,证明其中含有蛋白质,可能与其具有的免疫作用相关;野菊花出现在1 734和1 515cm-1等CO伸缩振动吸收峰,证明其中含有挥发油等酯类成分。由于二者的红外光谱具有较高的相似性且难以区分,通过二级鉴别比较闹羊花与野菊花的二阶导数红外光谱可看出,在1 656和1 515cm-1附近的吸收峰,表明二者均含有黄酮类成分;野菊花的二阶导数谱图中出现在1 163,1 077,1 026,986和869cm-1的吸收峰与菊糖的特征吸收峰一致,因此可以看出野菊花中含有菊糖。选取不同波数范围的闹羊花与野菊花的二维相关红外光谱进行对比,发现在1 700~1 400cm-1黄酮类成分区域闹羊花有3个明显的自动峰,野菊花有10个明显的自动峰;在1 250~900cm-1糖苷类成分区域闹羊花有10个明显的自动峰,野菊花有9个明显的自动峰。红外光谱的"三级鉴定法"为中药材的鉴别提供更快速、准确、方便的手段。     

基于网络药理学探讨玫瑰花抗抑郁物质基础及作用机制

利用网络药理学和分子对接方法探究玫瑰花抗抑郁的物质基础及作用机制。通过中国知网收集抗抑郁单体和玫瑰花的化学成分,借助PubChem、SwissTargetPrediction数据库预测玫瑰花的抗抑郁活性成分及作用靶点,通过DAVID数据库进行通路富集分析,运用Discovery Studio 2017软件对关键成分和靶点进行分子对接。收集抗抑郁单体117个,玫瑰花成分127个,筛选出玫瑰花与抗抑郁相关的核心成分17个,分子对接显示玫瑰花所含芹菜素、槲皮素、山柰酚、异丁香酚、异槲皮苷、矢车菊素-3-O-葡萄糖苷6个活性成分,可较好地与AKT1、PTGS2、ESR1 3个抑郁相关靶点结合。结果表明玫瑰花抗抑郁的物质基础为芹菜素、槲皮素、山柰酚等黄酮类化合物,主要通过影响HIF-1信号通路、神经活性配体-受体相互作用信号通路、催乳激素信号通路、多巴胺能神经突触信号通路发挥抗抑郁作用。该研究为抗抑郁新药研发提供了理论依据及新的研究思路。     

葛花总黄酮的抗氧化作用研究

为研究葛花总黄酮的体外抗氧化作用,以70%乙醇为溶剂,微波方法提取葛花中的总黄酮,用比色法测定其含量为4.72%;通过还原能力的测定、Fenton反应体系、DPPH法以及邻苯酚自氧化体系等评价葛花总黄酮体外抗氧化能力.结果显示,葛花总黄酮在还原力测定以及对三种自由基的清除上,表现出了不同程度的抗氧化能力.对O2-.和DPPH.及.OH 3种自由基具有明显的的清除作用,其EC50分别为:0.095mg/ml、0.114mg/ml、0.700mg/ml.葛花总黄酮具有较强的还原力,在清除自由基方面其清除率与其浓度存在着明显的量效关系.     

忍冬藤挥发油化学成分GC/MS分析

使用水蒸气蒸馏法提取忍冬藤中的挥发油,利用气相色谱-质谱联用技术对忍冬藤化学成分进行分离鉴定,采用色谱峰面积归一化法确定各成分的相对含量.分析结果表明,共分离出31种组分,鉴定了其中的15个组分,占挥发油组分总量的48.39%.     

微波法提取丁香色素

研究微波法提取丁香中食用色素的最佳工艺条件。方法：称取一定量的备用原料,选取微波功率、辐射时间、提取剂浓度、原料用量（g）与提取剂用量（mL）的配比（料液比）等进行单因素试验与正交试验。结果：微波功率是影响提取丁香色素的主要因素;影响丁香色素提取的顺序是微波功率〉料液比〉辐射时间〉提取剂浓度;最优工艺条件是微波辐射功率为500 W,辐射时间为120 s,提取剂为20%乙醇溶液,料液比为1 g：8 mL;提取液浓度与料液比之间存在交互作用。结论：正交试验是省时省力、结果易得的实用方法。     

动态微波辅助萃取与高效液相色谱联用测定金银花中的绿原酸

通过流动注射的方法将动态微波辅助萃取与高效液相色谱相连接, 用于测定金银花中的绿原酸. 萃取过程在一个循环体系中完成, 萃取后, 通过采样环采集到的20 μL样品被流动相载带到色谱系统进行分离检测. 在最佳实验条件下得到的检出限和测定下限分别为0.25和0.83 μg/mL, 日内和日间精密度(RSD)分别为3.4%和4.1%, 平均加标回收率为98.1%.     

金银花-连翘药对的成分和药理作用研究进展

配伍是中药临床用药的特色,药对是临床配伍的最小配伍单位,金银花-连翘药对是温病治疗中的常用药对,可以增强单味药物清热解毒、疏散风热的作用。本文从化学成分、药理药效作用方面对其进行了综述,为进一步研究金银花-连翘药对的作用机制、科学用药提供依据。