当归挥发油的提取与成分分析

采用常压水蒸汽蒸馏法、超声波提取法、微波提取法提取当归挥发油,实验表明采用微波提取法在微波功率720 W、萃取时间120 s、100 mL环己烷中的收率最高,为1.04%.并采用GC-MS联用技术对3种方法提取到的挥发油进行了成分和含量分析,主要成分是当归的活性成分藁本内酯.     

超临界CO2流体中藁本内酯可溶性压力估算及在当归油中的溶解度测定

从分子结构角度出发，首次估算了当归油中最主要成分藁本内酯的溶解度参数和在超临界CO2流体（SC—CO2）中的可溶性压力，从理论上预测了用SC—CO2萃取藁本内酯是可行的，并且40℃比50℃更有利。通过实验证实了理论估算的正确性，并指出在当归油体系中，由于其他成分的协同作用，藁本内酯在SC-CO2流体中的溶解能力得以提高。     

当归中藁本内酯的提取、分离与结构鉴定

运用超临界流体萃取法、水蒸气蒸馏法和有机溶剂提取法提取当归挥发油,运用硅胶柱分离纯化其主要成分藁本内酯并通过核磁共振进行结构鉴定.结果表明,超临界萃取法可以更好地提取当归挥发油,通过硅胶柱分离最终可得到纯度大于97%的藁本内酯,且为Z ligustilide.     

三步反应合成藁本内酯研究

以苯酞为起始原料,经3步反应,成功合成出了藁本内酯,研究了光照、温度、惰性气体保护等反应条件对产品产率和纯度的影响,并用HPLC-MS联用仪对产品进行了定性定量分析。结果表明,采用该方法合成藁本内酯三步反应的产率分别为:96%,68%,59%,总的反应产率为39%,得到目标产品纯度为94.39%;在合成和纯化的过程中采取低温、惰性气体保护、避光、选用石油醚-丙酮作为洗脱剂进行柱层析,可以减少副反应和产品异构化的发生,提高产品的产率和纯度。     

Separation and Purification of Z Ligustilide and Senkyunolide A from Ligusticum chuanxiong Hort. with Supercritical Fluid Extraction and High‐Speed Counter‐Current Chromatography

Abstract

The essential oil was obtained by supercritical fluid extraction from dried roots of Ligusticum chuanxiong. Different solvent systems for high‐speed counter‐current chromatography (HSCCC) were compared. A system composed of n hexane–ethyl acetate–methanol–water–acetonitrile in the ratio of 8:2:5:5:3 (v/v) was found to be optimum for HSCCC of the essential oil. Z ligustilide and senkyunolide A were separated by HSCCC with purity of 98% determined by GC. The chemical structures of these two components were identified by nuclear magnetic resonance (NMR) and mass spectrometry (MS).     

近红外光谱技术快速测定当归中藁本内酯含量

基于近红外光谱技术,运用偏最小二乘回归(PLSR)方法实现当归中藁本内酯含量的快速、无损检测.采用高效液相色谱(HPLC)法测定当归中藁本内酯含量,一阶导数结合正交信号校正对原始光谱进行预处理,建立当归近红外光谱和藁本内酯含量之间的最小二乘回归定量分析模型.结果表明:模型在校正集上的均方根误差(RMSEE)、交叉验证均方根误差(RMSECV)和决定系数R2分别为0.199 9,0.3489和0.9932,在预测集上的预测均方根误差(RMSEP)和决定系数R2分别为0.23和0.9941.方法具有简单、快速、不破坏样品等特点,可用于当归中藁本内酯含量的快速检测.     

Fermented Angelicae tenussimae with Aspergillus oryzae Improves Skin Barrier Properties,Moisturizing, and Anti-Inflammatory Responses

Angelicae tenussimae root has been used as a traditional medicine in Asia. Recently, anti-melanogenic and anti-photogenic effects of fermented A. tenuissima root (FAT) were identified. However, information about the anti-atopic dermatitis action of FAT is limited. Thus, the purpose of this study is to determine the applicability of FAT to AD by identifying the efficacy of FAT on the skin barrier and inflammatory response, which are the main pathogenesis of AD. Expression levels of skin barrier components and the production of inflammatory mediators in human keratinocyte and mouse macrophage cells were measured by quantitative RT-PCR or ELISA. FAT upregulated the expression of skin barrier components (filaggrin, involucrin, loricurin, SPTLC1) and inhibited the secretion of an inflammatory chemokine TARC in HaCaT cells. Furthermore, it suppressed pro-inflammatory cytokines (IL-6, TNF-α) and nitric oxide production in LPS-induced RAW264.7 cells. In addition, ligustilide increased filaggrin and SPTLC1, and also lowered pro-inflammatory mediators that increased in atopic environments, such as in FAT results. This means that ligustilide, one of the active ingredients derived from FAT, can ameliorate AD, at least in part, by promoting skin barrier formation and downregulating inflammatory mediators. These results suggest that FAT is a potential functional cosmetic material for the care and management of AD.     

当归胶囊中三种有效成分含量测定的方法学验证

目的:建立当归胶囊中三种有效成分藁本内酯、阿魏酸、粗多糖的含量测定方法,并对检测方法进行方法学验证。方法:藁本内酯、阿魏酸采用高效液相色谱法,粗多糖采用紫外分光光度法,进行系统适应性、专属性、线性、检出限、准确度、精密度、重复性、稳定性等的方法学考察。结果:藁本内酯在20~60 μg/mL线性良好,r=0.9996,平均加样回收率为99.72%(RSD=2.99%),精密度、重复性、稳定性RSD均≤1%;阿魏酸在6~18 μg/mL线性良好,r=0.9990,平均加样回收率为96.11%(RSD=4.18%),精密度、重复性、稳定性RSD均≤2%;粗多糖在0.05~0.15 mg线性良好,r=0.9987,平均加样回收率为103.52%(RSD=4.79%),精密度、重复性、稳定性RSD均≤5%。结论:三种方法准确、可靠,可用于当归胶囊中三种有效成分藁本内酯、阿魏酸、粗多糖的含量测定。     

鱼腥草多酚对葡聚糖硫酸钠（DSS）诱导小鼠溃疡性结肠炎的改善作用

目的：探究蒿本内酯（ligustilide,Lig）对葡聚糖硫酸钠（dextran sodium sulfate,DSS）诱导溃疡性结肠炎（ulcerative colitis,UC）小鼠的改善作用及机制。方法：将60只雄性SPF级C57BL/6小鼠随机分成6组,分别为空白组、DSS组、阳性药柳氮磺吡啶（sulfasalazine,SASP）组、Lig低、中、高剂量组。DSS组小鼠自由饮用3% DSS水溶液7 d复制UC模型,同时对Lig低、中、高剂量组小鼠灌胃给予药物干预治疗。通过记录小鼠每日体重和结肠长度,检测疾病活动指数（disease activity index,DAI）评分,采用酶联免疫吸附测定试剂盒定量检测血清中TNF-α、IL-6和IL-1β的表达水平,检测结肠中TLR4/NF-κB蛋白表达水平,并结合苏木素-伊红染色实验,探究Lig对小鼠UC的作用及机制。结果：与空白组比较,DSS组小鼠体重显著减轻（P<0.05）,结肠长度显著缩短（P<0.05）,DAI评分显著升高（P<0.05）,肠道出现大量炎症性浸润现象,且结肠组织中TNF-α、IL-6和IL-1β表达水平显著升高（P<0.05）;与DSS组比较,Lig中剂量组和高剂量组小鼠的肠道组织中TNF-α、IL-6和IL-1β的表达以及TLR4/NF-κB信号均被显著抑制（P<0.05）,表明Lig中剂量组和高剂量组小鼠肠道损伤得到显著改善。结论：Lig能有效改善DSS诱导的小鼠UC,其机制可能是抑制NF-κB信号通路的激活。

     

川芎主要药理活性成分药理研究进展

川芎含有超过100种药理活性成分，本文基于其主要生物活性成分药代动力学的研究，重点对川芎中的阿魏酸、藁本内酯、洋川芎内酯A、洋川芎内酯I及川芎嗪等成分的体内过程和药理作用的最新研究进展进行综述，以期为川芎的临床应用及深度开发利用提供一些新的思路与方法。