酸橙和甜橙2种枳实药材HPLC指纹图谱研究及其柚皮苷和辛弗林含量分析

目的:研究酸橙和甜橙2种枳实药材的高效液相色谱(HPLC)指纹图谱并测定药材中柚皮苷和辛弗林的含量,以建立枳实药材有效的质量评价方法。方法:采用高效液相色谱(HPLC)法建立指纹图谱和测定有效成分含量,对来自20个产地的2个种的枳实药材进行分析。色谱柱为AlltimaC18(250mm×4.6mm,5μm),流动相为乙腈-水(含0.1%磷酸或加上0.1%十二烷基硫酸钠),流速为1.0mL·min-1,指纹图谱检测波长为224nm,柚皮苷和辛弗林含量测定的检测波长分别为283、224nm。结果:得到分离度、重复性均较好的枳实药材HPLC指纹图谱。对20批不同产地枳实药材(包含2个种)HPLC指纹图谱的相似度评价结果显示,酸橙和甜橙2种枳实的指纹图谱差异显著,但同种枳实中不同产地的差异不大;含量测定结果显示,不同产地和不同种枳实药材中柚皮苷和辛弗林含量差异较大。结论:该方法简便、准确、灵敏度高、重复性好,可作为枳实药材的质量控制方法,此方法已被《香港中药材标准》采用。不同种和产地的枳实药材有效成分(柚皮苷和辛弗林)的含量具有明显差异,临床处方应当区别应用。     

四大主产区枳壳的指纹图谱分析

摘要：目的:建立枳壳色谱指纹图谱的分析方法,评价四个主产区枳壳药材的质量属性,并基于聚类分析和主成分分析方法,为不同主产区枳壳药材质量控制提供参考。方法:采用Agilent ZORBAX SB-C18（4.6 mm×250 mm, 5μm）色谱柱,以甲醇（A）-水（B）为流动相梯度洗脱,流速：1.0ml·min-1,检测波长：330 nm,柱温：30℃,建立14批次四大主产区枳壳的HPLC指纹图谱,比较四大主产区枳壳指纹图谱的相似度,并应用SPSS19统计软件对四大主产区枳壳进行聚类分析和主成分分析,综合评价四大主产地枳壳药材的质量。结果:枳壳药材HPLC指纹图谱16个峰确定为共有峰,并指认了2号峰为柚皮苷,3号峰为新橙皮苷,9号峰为木犀草素,14批次四大主产区枳壳指纹图谱和对照图谱的相似度为0.873～0.972;聚类分析及主成分分析显示不同主产区枳壳间存在一定的差异。结论:建立的枳壳指纹图谱重现性及专属性较好,聚类分析及主成分分析较好地解释了不同主产区枳壳药材的质量差异,为枳壳药材的质量控制提供科学的参考。     

不同产地枳实与枳壳中黄酮类成分的含量测定

目的:建立枳实、枳壳药材中橙皮苷、柚皮苷等四种黄酮类成分的含量测定方法,并比较此类成分在两种药材中的区别。方法:采用反相高效液相色谱法,用Inertsil ODS(250×4.6mm,5μm)色谱柱,以甲醇-水-冰醋酸(38:58:4)为流动相;流速为1.0mL·mim~(-1);柱温为35℃;检测波长为284nm。结果:枳实中主要含橙皮苷、芸香柚皮苷,而枳壳中以新橙皮苷和柚皮苷含量较高;且枳实中总黄酮含量高于枳壳。结论:黄酮类成分的种类和含量高低均有很大区别,揭示产地、品种以及采收期的不同影响其含量分布。     

广西地不容药材的HPLC指纹图谱研究

目的:建立广西地不容药材的高效液相色谱(HPLC)指纹图谱。方法:采用HPLC法。色谱柱为Hypersil ODS2,流动相为乙腈-0.5%磷酸溶液(梯度洗脱),流速为1.0 m L/min,检测波长为282 nm,柱温为30℃,进样量为10μL。以延胡索乙素为参照,测定10批药材样品的HPLC图谱,采用《中药色谱指纹图谱相似度评价系统》(2012版)进行共有峰指认和相似度评价。结果:10批广西地不容的HPLC图谱有17个共有峰,10批药材样品中有8个产地药材指纹图谱与对照图谱比较相似度>0.900,2个产地药材相似度<0.900。结论:该研究所建HPLC指纹图谱可为广西地不容的鉴别和质量评价提供参考;广西区内多数产地的地不容药材所含生物碱类成分相似,少数存在差异。     

骨碎补药材HPLC指纹图谱的构建及质量控制

目的建立骨碎补药材HPLC指纹图谱分析方法、控制其产品质量。方法以抽皮苷和新北美圣草苷为对照品,建立骨碎补HPLC指纹图谱法,测定全国不同产地10批骨碎补样品。色谱条件:色谱柱lichrospher C18(250mm×4.6mm,5μm),甲醇-0.1%磷酸水为流动相进行梯度洗脱,流速1.0mL/min,柱温25℃,检测波长为283nm。结果建立了骨碎补药材的HPLC指纹图谱,抽皮苷和新北美圣草苷的平均回收率分别为101.6%和97.6%,RSD分别<4.5%和5.0%。标定了8个共有峰,鉴别了真伪骨碎补。结论利用HPLC指纹图谱可以比较全面控制骨碎补药材的内在质量。     

蕲艾的HPLC指纹图谱研究

目的:建立蕲艾的高效液相色谱(HPLC)指纹图谱。方法:采用HPLC法。色谱柱为ZORBAX Extend-C18,流动相为乙腈-0.2%磷酸水溶液(梯度洗脱),检测波长为330 nm,流速为1.0 ml/min,柱温为30℃。以柚皮苷为参照物,对10批蕲艾样品进行指纹图谱分析,并利用《中药色谱指纹图谱相似度评价系统》对所得数据进行相似度评价。结果:10批蕲艾样品共标定12个共有峰,共指认出3个共有峰,分别为绿原酸、柚皮苷、山柰酚;10批药材的相似度>0.90。结论:所建立的指纹图谱可用于蕲艾药材的品质评价和质量控制。     

河南产山橿醋酸乙酯部位HPLC指纹图谱研究

目的 建立山橿醋酸乙酯部位的HPLC色谱指纹图谱。方法 采用高效液相色谱法,色谱条件：依利特Hypersil ODS2 C₁₈(250 mm×4.6 mm,5 μm)色谱分析柱;流动相：甲醇-水梯度洗脱;检测波长297 nm;柱温30 ℃;流速1.0 mL·min^-1。结果 本试验在测定了23批山橿药材醋酸乙酯部位的HPLC色谱指纹图谱的基础上,建立了山橿药材醋酸乙酯部位的HPLC色谱指纹图谱,并进行了相似度分析,除了河南省西峡县产山橿药材的相似度比较低外,其余相似度都在0.85以上。结论 本方法简便、快捷、可靠,可用于山橿药材的质量控制。     

不同产地甘草药材高效液相色谱指纹图谱研究

目的采用高效液相色谱法建立不同产地甘草药材的指纹图谱。方法采用Hypersil ODS2 C18 （4.6 mm×250 mm,5 μm）色谱柱,甲醇 0.1%磷酸水溶液为流动相梯度洗脱,流速为0.6 mL&#8226;min 1,检测波长254 nm,采集时间90 min。结果得到了分离度较好的甘草药材高效液相色谱指纹图谱,标定出了11个共有指纹峰,方法学考察结果符合指纹图谱技术要求。结论确定的指纹图谱研究方法稳定、可靠,可用于甘草药材的质量控制。     

竹叶柴胡药材HPLC指纹图谱研究

目的:建立竹叶柴胡药材的高效液相色谱指纹图谱。方法:色谱柱为Agilent C1(8250mm×4.6mm,5μm),流动相为乙腈-0.2%磷酸水溶液(梯度洗脱),流速为1.0mL·min-1,柱温为30℃,检测波长为203nm。结果:建立了竹叶柴胡药材的指纹图谱,确定了22个共有峰,各峰的相似度均>0.800。结论:该指纹图谱建立方法简单、重复性好,可为竹叶柴胡药材的鉴别和质量评价提供参考。     

基于玉屏风煎剂的玉屏风制剂质量评价研究

目的:测定玉屏风制剂中毛蕊异黄酮苷、升麻素苷、5-O-甲基维斯阿米醇苷的含量并分析其高效液相色谱(HPLC)指纹图谱,以玉屏风煎剂的内在质量评价不同厂家、不同剂型玉屏风制剂的质量。方法:采用HPLC法测定3种成分的含量,色谱柱为Hypersil ODS(250mm×4.6mm,5μm),流动相为乙腈-水(梯度洗脱),检测波长为254nm,流速为1mL·min-1,柱温为30℃。采用HPLC法分析指纹图谱,色谱柱为Hypersil ODS(250mm×4.6mm,5μm),流动相为乙腈-水(梯度洗脱),检测波长为220nm,流速为1mL·min-1,柱温为30℃。结果:按日用量计,颗粒剂中3种成分的含量均>口服液的含量,提示玉屏风不同剂型因工艺不同,其有效成分的保留有较大差异;颗粒剂含量基本高于煎剂含量,与煎剂煎煮2次提取率不高的结果基本相符。3个不同厂家口服液指纹图谱共有模式的相似度只在0.830～0.942之间,表明同剂型不同厂家之间产品质量有较大差异;颗粒剂共有模式与口服液共有模式之间的相似度仅为0.899;与煎剂指纹图谱相比,颗粒剂共有模式的相似度为0.964,3个药厂口服液模式的相似度分别为0.929、0.799、0.935,提示颗粒剂的质量与传统煎剂质量较为接近,与含量测定结果基本相符。结论:玉屏风制剂水提工艺基本能保留原煎剂的化学物质基础;基于玉屏风煎剂质量的玉屏风制剂质量评价的方法,可以为制剂工艺合理性与临床用药指导提供一定的参考。     

Nachweis einiger Heilmittel in der Kniegelenksynovialflüssigkeit

Zusammenfassung Mittels Gaschromatographie und Dünschichtchromatographie wiesen die Autoren 11 Substanzen nach, welche durch Injektion oder nach Verabreichung per os in die Kniegelenksynovialflüssigkeit eindrangen. In ihrer Aufstellung konnten sie eine direkte Beziehung zwischen Struktur sowie chemischphysikalischen Eigenschaften der Substanz und ihrer Fähigkeit, aus dem Blut in die Kniegelenksynovialflüssigkeit einzudringen, nicht nachweisen, außer der Tatsache, daß Substanzen mit starker Affinität zu Eiweißstoffen erst in höheren Dosen nachweisbar waren.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

Emerging drugs for epilepsy

Epilepsy affects ≤ 1% of the world's population. Antiepileptic drugs (AEDs) are the mainstay of treatment, although more than a third of patients are not rendered seizure free with existing medications. Uncontrolled epilepsy is associated with increased mortality and physical injuries, and a range of psychosocial morbidities, posing a substantial economic burden on individuals and society. Limitations of the present AEDs include suboptimal efficacy and their association with a host of adverse reactions. Continued efforts are being made in drug development to overcome these shortcomings employing a range of strategies, including modification of the structure of existing drugs, targeting novel molecular substrates and non-mechanism-based drug screening of compounds in traditional and newer animal models. This article reviews the need for new treatments and discusses some of the emerging compounds that have entered clinical development. The ultimate goal is to develop novel agents that can prevent the occurrence of seizures and the progression of epilepsy in at risk individuals.     

盐酸达泊西汀中甲磺酸甲酯、甲磺酸乙酯及甲磺酸异丙酯的顶空毛细管GC-ECD法测定

建立了衍生化顶空毛细管气相色谱-电子捕获检测器(ECD)法测定盐酸达泊西汀中的甲磺酸甲酯(MMS)、甲磺酸乙酯(EMS)和甲磺酸异丙酯(IMS).应用碘化钠衍生技术,使用PW-5毛细管柱,载气为氮气,ECD检测,程序升温.MMS、EMS和IMS分别在0.03～0.30、0.05～0.50和0.05～0.50 μg/ml浓度范围内线性关系良好,平均回收率分别为63.5％、100.3％和96.2％,最低检测限分别为0.30、0.50和0.50 ng/ml.     

Lung disease and PKCs

The lung offers a rich opportunity for development of therapeutic strategies focused on isozymes of protein kinase C (PKCs). PKCs are important in many cellular responses in the lung, and existing therapies for pulmonary disorders are inadequate. The lung poses unique challenges as it interfaces with air and blood, contains a pulmonary and systemic circulation, and consists of many cell types. Key structures are bronchial and pulmonary vessels, branching airways, and distal air sacs defined by alveolar walls containing capillaries and interstitial space. The cellular composition of each vessel, airway, and alveolar wall is heterogeneous. Injurious environmental stimuli signal through PKCs and cause a variety of disorders. Edema formation and pulmonary hypertension (PHTN) result from derangements in endothelial, smooth muscle (SM), and/or adventitial fibroblast cell phenotype. Asthma, chronic obstructive pulmonary disease (COPD), and lung cancer are characterized by distinctive pathological changes in airway epithelial, SM, and mucous-generating cells. Acute and chronic pneumonitis and fibrosis occur in the alveolar space and interstitium with type 2 pneumocytes and interstitial fibroblasts/myofibroblasts playing a prominent role. At each site, inflammatory, immune, and vascular progenitor cells contribute to the injury and repair process. Many strategies have been used to investigate PKCs in lung injury. Isolated organ preparations and whole animal studies are powerful approaches especially when genetically engineered mice are used. More analysis of PKC isozymes in normal and diseased human lung tissue and cells is needed to complement this work. Since opposing or counter-regulatory effects of selected PKCs in the same cell or tissue have been found, it may be desirable to target more than one PKC isozyme and potentially in different directions. Because multiple signaling pathways contribute to the key cellular responses important in lung biology, therapeutic strategies targeting PKCs may be more effective if combined with inhibitors of other pathways for additive or synergistic effect. Mechanisms that regulate PKC activity, including phosphorylation and interaction with isozyme-specific binding proteins, are also potential therapeutic targets. Key isotypes of PKC involved in lung pathophysiology are summarized and current and evolving therapeutic approaches to target them are identified.