麻黄与杏仁混合汤剂红外光谱分析

测试了单味药麻黄、杏仁及麻黄+杏仁混合汤剂的红外光谱。经分析：在麻黄+杏仁汤剂中保留了麻黄、杏仁单味药物汤剂中的某些吸收峰,见麻黄+杏仁光谱1 402和1 076 cm-1处等;麻黄、杏仁光谱中的某些吸收峰并未在麻黄+杏仁光谱中出现,见麻黄+杏仁光谱1 394和682 cm-1处等;在麻黄+杏仁汤剂光谱中,出现了新的吸收峰,见麻黄+杏仁光谱688和1 187 cm-1处等。同时,因吸收峰位置的改变,说明各基团在麻黄、杏仁、麻黄+杏仁汤剂中所处的化学环境不同, 汤剂中生化物质的结构发生了变化,或麻黄+杏仁汤剂中可能新生成了麻黄、杏仁单味药物汤剂中所没有的化学成分。麻黄+杏仁汤剂所包含的药物成分并非是单味麻黄、杏仁汤剂所含药物成分的简单相加。     

茵陈蒿汤对肝纤维化大鼠Caspase-12通路以及TIMP-1、Smad2的影响

目的探究茵陈蒿汤对肝纤维化（LF）大鼠Caspase-12通路以及TIMP-1、Smad2的影响。方法雄性SD大鼠45只,随机分为3组,即对照组,模型组和茵陈蒿汤组。使用腹腔注射CCl 4 建立LF模型,茵陈蒿汤组在建模时使用茵陈蒿汤灌胃,持续8周。比较8周后各组大鼠的一般情况,分别使用HE染色和Masson染色观察肝组织形态和纤维化情况。分别使用Western blot和RT-qPCR检测蛋白和mRNA的水平。结果模型组大鼠出现明显的肝损伤和纤维化,茵陈蒿汤组大鼠肝损伤情况和纤维化情况显著减轻。血生化结果显示,模型组ALT和AST水平显著高于对照组（P <0. 05）,菌陈蒿汤干预后ALT和AST水平显著低于模型组,差异具有统计学意义（P <0. 05）。建模后8周模型组大鼠肝组织中GRP78、eIF2α和Caspase-12显著升高（P <0. 01）,茵陈蒿汤组的GRP78、eIF2α和Caspase-12显著低于模型组（P <0. 01）。模型组的Collagen Ⅰ、Collagen Ⅲ、TIMP-1、Smad2 mRNA和蛋白水平显著高于对照组（P <0. 01）,茵陈蒿汤组Collagen Ⅰ、Collagen Ⅲ、TIMP-1、Smad2 mRNA和蛋白水平显著低于模型组（P <0. 01）。结论茵陈蒿汤可显著缓解大鼠肝组织的纤维化,这可能由于茵陈蒿汤具有抑制Caspase-12通路以及Smad2基因的表达发挥抗纤维化和抗凋亡的作用有关。     

Separation and identification of multiple constituents in Xiao Chai Hu Decoction (Sho‐saiko‐to) by bioactivity‐guided fractionation combined with LC‐ESI‐QTOFMS/MS

Xiao Chai Hu Decoction (XCHD), named Sho‐saiko‐to in Japanese, is a well‐known traditional Chinese medicine formula used in Asia. However, the characterization methods used in the past have lacked sensitivity and the nature of the active constituents of XCHD remains unclear. This study was carried out to establish the hyphenated method of bioactivity‐guided fractionation and liquid chromatography coupled with electrospray ionization quadrupole time‐of‐flight mass spectrometry (LC‐ESI‐QTOFMS/MS) in order to identify the major bioactive constituents of XCHD. D101 macroporous resin was used to separate and enrich the material base into four fractions, XCHD‐1, XCHD‐2, XCHD‐3 and XCHD‐4. Each fraction was then evaluated for its antidepressant effect using depression‐related parameters. An LC‐ESI‐QTOFMS/MS method in both positive and negative ion mode was also applied for separation and identification of the biological active fractions of XCHD. As a result, 79 compounds including polysaccharides, flavonoids, saikosaponins, ginsenosides, licoricesaponins and gingerols were detected, 69 of them were identified or tentatively characterized. Based on our preliminary characterization investigations, polysaccharides, gingerols and flavonoids in XCHD may contribute to the antidepressant effect of XCHD. In conclusion, the hyphenated method of bioactivity‐guided fractionation and LC‐ESI‐QTOFMS/MS was meaningful for the isolation and preliminary identification of the biological active components in complex matrices of traditional Chinese medicine. Copyright © 2014 John Wiley & Sons, Ltd.     

Chemical profiling of Qingfei Paidu Decoction by triplex off-line two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

Qingfei Paidu Decoction is a Chinese medicine formula that has been proved effective in the treatment of coronavirus disease 2019. However, the comprehensive separation and characterization of Qingfei Paidu Decoction are of a great challenge due to the diversity of chemical components in a wide range of polarity. In this study, a triplex off-line two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry is developed for the analysis of Qingfei Paidu Decoction. One reversed-phase liquid chromatography×hydrophilic interaction liquid chromatography system and two reversed-phase liquid chromatography×reversed phase liquid chromatography systems were constructed to separate polar components and weak-polar components in Qingfei Paidu Decoction, respectively. Benefiting from the good orthogonality of two-dimensional liquid chromatography and high sensitivity of quadrupole time-of-flight MS, chemical components with different polarities and content were discovered. A total of 749 peaks were detected in positive and negative ionization mode and presented as a four-dimensional data plot. Meanwhile, 498 compounds belonging to 14 categories were tentatively identified. These results provide good supplementary to elucidate the material basis of Qingfei Paidu Decoction. The triplex off-line two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry strategy can be a powerful and efficient tool for the separation and characterization of chemical substances in traditional Chinese medicine formulas.     

An enhanced analytical strategy integrating offline two-dimensional liquid chromatography with high-resolution accurate mass spectrometry and molecular networking: Comprehensive characterization of HuangLian JieDu Decoction as a case study

Comprehensive ingredient research is of great significance for understanding the effective material basis of herbal medicines, but due to the diversity and complexity of their phytochemicals, such research is challenging. Here, a multifaceted strategy was proposed to analyze and identify the composition of HuangLian JieDu Decoction based on offline two-dimensional liquid chromatography combined with ultraviolet detection and high-resolution mass spectrometry. Multiple components were separated by two-dimensional liquid chromatography, which consisted of hydrophilic interaction chromatography and reversed-phase liquid chromatography, and then further characterized by high-resolution mass spectrometry with a full mass spectrometry/precursor ion list/data-dependent secondary scan data acquisition method. For data processing, database screening and molecular networking were used to identify the components in HuangLian JieDu Decoction. The offline two-dimensional liquid chromatography combined with ultraviolet detection and a high-resolution mass spectrometry system showed good orthogonality of 76.35% and a high peak capacity of 5175, effectively separating multiple components. Finally, 527 compounds, including 164 alkaloids, 133 terpenoids, 88 flavonoids, 60 phenylpropanoids, 38 organic acids, and 44 other compounds, were characterized. This integrated approach is suitable for the comprehensive characterization of herbal medicines and other complex chemical systems.     

HPLC-DLS法表征麻杏石甘汤中甘草酸成分

研究麻杏石甘汤煎煮过程中甘草酸质量浓度的变化及其聚集状态.采用Daisogel-C18色谱柱(250 mm×4.6mm,5μm),流动相甲醇-0.2 mol·L-1醋酸铵溶液-冰醋酸体积比为67∶33∶1,在流速为1.0 m L·min-1,柱温为25℃条件下检测不同煎煮时间、超滤前后麻杏石甘汤中甘草酸质量浓度变化.联用Zetasizer粒度仪考察麻杏石甘汤中甘草酸的存在形式.结果表明,麻杏石甘汤煎煮过程中前20 min甘草酸质量浓度显著上升,随后无明显变化.超滤前麻杏石甘汤中颗粒平均粒径约为250.0 nm,甘草酸质量浓度约82.4μg·m L-1,超滤后无明显颗粒,甘草酸质量浓度极小.从而得出结论:麻杏石甘汤煎煮过程中,甘草酸从药材释放到汤剂中,并通过超分子作用自身或与其它化学成分形成胶束而存在于汤剂中.     

黄连解毒汤的药理作用及其在兽医上的临床应用

黄连解毒汤有清热解毒、镇痛、止血、抗菌、抗炎等药理作用,为清热解毒的代表方剂.本文将黄连解毒汤药理作用和兽医临床应用作一概述.     

气相色谱法测定黄芪饮片中有机氯类农药残留

采用气相色谱电子捕获检测器(ECD)测定黄芪饮片中9种有机氯类农药残留。黄芪饮片样品以丙酮、二氯甲烷提取,浓硫酸磺化,采用HP–5(30 m×0.32 mm,0.25μm)色谱柱,气化室温度为250℃,检测器温度为300℃。以标准曲线法计算农药含量,加标回收率为94.5%~104.4%,测定结果的相对标准偏差为1.7%~2.7%,检出限为0.061~0.175 ng/m L。该方法简单、快速、稳定、可靠,可用于黄芪饮片中9种有机氯类农药残留的测定。     

Simultaneous quantification of five anthraquinones in rat plasma by high-performance liquid chromatography with fluorescence detection

A sensitive high-performance liquid chromatographic method with fluorescence detection (excitation 435 and emission 515 nm) was established and validated for quantification of five anthraquinones (aloe-emodin, rhein, emodin, chrysophanol and physcion) in rat plasma. Following a single-step liquid-liquid extraction, the analytes and internal standard (1,8-dihydroxyanthraquinone) were separated on a reversed-phase C(18) column with water-phosphoric acid-methanol as mobile phase at a flow rate of 1 mL/min. The linear ranges of the calibration curves were 6.5-1300 ng/mL for aloe-emodin, 20-4000 ng/mL for rhein, 40-8000 ng/mL for emodin, 15-3000 ng/mL for chrysophanol and 13-2600 ng/mL for physcion. The lower limit of quantification was 6.5 ng/mL for aloe-emodin, 20 ng/mL for rhein, 40 ng/mL for emodin, 15 ng/mL for chrysophanol and 13 ng/mL for physcion. The mean accuracy was 94.3-105.1% for aloe-emodin, 90.3-108.8% for rhein, 92.6-106.7% for emodin, 95.8-103.8% for chrysophanol and 98.7-101.2% for physcion. The within-batch and between-batch precisions were < or = 5.5% and < or = 13.4%, respectively. This method is suitable for determining the five anthraquinones in plasma simultaneously and thus investigating the pharmacokinetics of anthraquinones from Xiexin decoction in rats.