高效液相色谱法测定不同产地假蒟中的α-细辛脑含量

目的 采用高效液相色谱（HPLC）法测定不同产地假蒟中α-细辛脑的含量。方法 色谱柱为Lichrospher C₁₈柱（150 mm×4.6 mm,5 μm）,流动相为乙腈-0.05%磷酸溶液（47：53）,流速为1.0 ml/min,检测波长313 nm,柱温30℃。结果 α-细辛脑在0.0970~1.934 μg范围内与峰面积有良好线性关系（r=0.999 8）,平均回收率为99.94%（RSD=1.13%）,样品在24 h内稳定,且该方法重复性较好。结论 本方法简便准确,可用于假蒟药材中α-细辛脑的含量测定,以控制其质量;我国不同产地的假蒟中α-细辛脑含量有明显差异,其中以广西产假蒟含量最高。     

HPLC法测定α-细辛脑PLGA原位凝胶中α-细辛脑的含量

目的:建立测定α-细辛脑聚乳酸-羟基乙酸共聚物(PLGA)原位凝胶中α-细辛脑含量的方法。方法:采用高效液相色谱法。色谱柱为SHIM-PACK VP-ODS(250mm×4.6mm,5μm),流动相为甲醇-水(75:25),检测波长为258nm,流速为1.0mL·min-1,柱温为30℃。结果:α-细辛脑的检测浓度在10.4～104.0μg·mL-1范围内与峰面积积分值呈良好线性关系(r=0.9999);平均加样回收率为95.83%,RSD=2.47%(n=9)。结论:本方法准确、可靠、稳定,可用于α-细辛脑PLGA原位凝胶的质量控制。     

GC-MS分析广西产4种栽培胡椒属植物叶中的挥发油成分

目的 分析小毛萎、假蒟、荜茇和山蒟4种植物叶中的挥发油成分.方法 采用GC-MS技术进行分析.结果 挥发油的得率较高,成分较为复杂,既有相同的主要化学成分,也有特异性成分.结论 主要成分的差异,能作为品种鉴别的依据.另外,假蒟中的α-细辛脑含量较高,值得关注.     

α-细辛脑注射乳含量测定方法研究

目的建立α-细辛脑注射乳含量测定方法。方法色谱柱为迪马C18柱(250mm×4.6mm,5μm);流动相为甲醇-水(70∶30);检测波长为258nm;流速1.0 mL/min;柱温30℃;进样量20μL。结果α-细辛脑2.01～80.40μg/mL质量浓度范围内线性关系良好,r=0.9999(n=6),平均回收率为99.74%,RSD为0.72%。结论方法操作简便,结果准确,可用于该品种的质量控制。     

HPLC测定热熔压敏胶贴剂中α-细辛醚的含量

目的建立HPLC测定热熔压敏胶贴剂中α-细辛醚含量的方法。方法以甲苯为萃取溶剂提取药物,采用ZORBAXEclipse XDB-C18色谱柱(150 mm×4.6 mm,5μm),以甲醇-水(55∶45)为流动相,流速:1.0 mL.min 1,检测波长:311 nm,柱温:40℃。结果α-细辛醚在8.032~18.07μg.mL 1内线性关系良好(r=0.999 9),回收率为99.3%(RSD=0.99%),供试品溶液在室温下48 h内稳定。结论本方法操作简单,结果准确,可用于热熔压敏胶贴剂中α-细辛醚的含量测定。     

高效液相色谱法测定细辛脑及其制剂的含量

目的:建立高效液相色谱法测定α-细辛脑及其制剂的含量。方法:色谱柱Diamonsil ODS-C18柱(200 mm×4．6 mm,5μm),流动相为甲醇-水(70:30),检测波长258 nm。结果:在20-100μg·ml-1浓度范围内呈良好的线性关系γ=0．999 8,平均回收率为99．8％,RSD=0．4％。结论:该法具有操作简便,快速,重现性好,结果准确的优点。     

反相高效液相色谱法测定α-细辛脑的含量及有关物质

目的:应用高效液相色谱法测定细辛脑原料药的含量及有关物质。方法:使用 Diamonsil C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-水(60:40),流速为1.0 mL·min~(-1),检测波长为258 nm。结果:α-细辛脑浓度在21.04～126.24μg·mL~(-1)范围内与峰面积呈良好线性关系(r=0.9999),平均回收率为99.42%(n=9)。结论:测定方法简便,准确性、专属性好,可用于质量控制。     

α-细辛脑脂质体的制备与体外释放药物的考察

目的 研究α-细辛脑脂质体的制备工艺,测定脂质体中α-细辛脑的体外释放度.方法 采用乙醇注入法制备α-细辛脑脂质,正交试验设计优化制备工艺,分光光度法测定α-细辛脑的含量.结果 最优工艺为磷脂浓度5％、磷脂与胆固醇的重量比8∶1、磷脂与药物的重量比50∶1,包封率为66.25％±0.21％,体外释放符合双相动力学方程Q=92.63-51.81exp(-2.89t)-40.82exp(-0.62t).结论 采用乙醇注入法制备α-细辛脑脂质,获得脂质体制备工艺.     

超滤-HPLC法测定α-细辛脑脂微球包封率

目的对α-细辛脑脂微球进行质量评价,测定α-细辛脑脂微球包封率。方法采用超滤法分离脂微球与游离药物;采用Diamonsil ODS柱(200 mm×4.6 mm,5μm),流动相为甲醇-水(70∶30),流速为1.0 mL/min,检测波长为258 nm,测定药物含量,计算包封率。结果α-细辛脑在1.6～8.0 mg/L内线性关系良好,超滤法能很好地将脂微球与游离药物分离,游离药物的平均回收率为99.96%,超滤回收率为99.56%,三批样品平均包封率为98.52%。结论该方法可用于α-细辛脑脂微球质量控制与包封率的测定。     

气相色谱法测定细辛脑注射液的含量

目的建立毛细管气相色谱法测定细辛脑注射液的含量。方法色谱柱为TR-1二甲基聚硅氧烷柱(30 m×0.25 mm,0.5μm),检测器为氢火焰离子化检测器(FID),柱温160℃。结果细辛脑注射液的浓度在0.100 4~5.020 mg·m L-1(r=0.999 6)范围内线性关系良好,平均回收率为99.1%(n=9)。结论建立的方法快速、简单,重复性好,可用于细辛脑注射液的质量控制。     

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.     

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.     

血管内皮生长因子的异常与子(癎)前期发病的关系

目的:研究血浆可溶性细胞间黏附分子-1(sICAM-1)浓度和胎盘组织血管内皮生长因子(VEGF)、胎盘生长因子(PLGF)及其血管内皮生长因子受体1(VEGFR1,Flt-1)、可溶性血管内皮生长因子受体1(sVEGFR1,sFlt-1)mRNA的表达与子前期的关系.方法:采用酶联免疫吸附测定法(ELISA)检测45例子前期患者和45例健康产妇血清sICAM-1的浓度,逆转录-聚合酶链反应(RT-PCR)方法检测胎盘组织中VEGF、PLGF、Flt-1、sFlt-1 mRNA的表达.结果:(1)子前期组sICAM-1水平为(218.45±29.93) μg/L,显著高于对照组的(168.84±19.39) μg/L(P < 0.01).(2)子前期患者胎盘组织VEGF、PLGF、Flt-1、sFlt-1 mRNA的相对表达量显著高于对照组(均P < 0.01).(3)血清sICAM-1浓度与胎盘组织中sFlt-1mRNA的相对表达量呈正相关(r = 0.90,P < 0.01).结论:子前期患者血清sICAM-1浓度升高,其胎盘组织VEGF、PLGF、Flt-1、sFlt-1 mRNA的相对表达量也升高.胎盘组织sFlt-1mRNA的高表达与子前期内皮损伤等有密切关系.     

Antiparasitic protozoan vaccines

Parasitic infections caused by pathogenic protozoa affect over 1 billion people worldwide and impose a substantial health and economic burden, particularly on inter-tropical less-developed countries where they are more prevalent. Despite encouraging progress in vaccine development, chemotherapy remains the single most effective, efficient and inexpensive means to control most parasitic infections [1]. However, day to day parasites are becoming increasingly resistant to drugs currently in use, such as Plasmodium towards chloroquine, lending to the start of a promising future for vaccines. Patent applications regarding vaccines for the prevention, control and diagnosis of parasitic protozoan infections are reviewed for the period December 1996 - October 2000. However, vaccines for some of the protozoan infections do not appear in the literature in the period reviewed; only, vaccines against malaria, leishmaniasis, trypanosomiasis, cryptosporidiosis, pneumocystosis, eimeriosis, toxoplasmosis and neosporosis, as well as Babesia microti infections have been found.     

Binding affinity in drug design: experimental and computational techniques

ABSTRACT

Introduction: In pharmaceutical design where future drugs are developed by targeting a specific chosen protein, the evaluation of ligand affinity is crucial. For this very purpose are a multitude of diverse methods which are continuously being improved, which, in turn, makes it difficult to choose which techniques to use in practice.

Areas covered: In this review, the authors discuss both experimental and computational approaches for affinity evaluation. Basic principles, general limitations and advantages, as well as main areas of application in drug discovery, are overviewed for some of the most popular ligand binding assays. The authors further provide a guide to affinity predictions, collectively covering several techniques that are used in the first stages of rational drug design.

Expert opinion: All affinity estimation methods have limitations and advantages that partially overlap and complement one another. Some of the suggested best practices include cross-verification of data using at least two different techniques and careful data interpretation.