HPLC法测定乙肝灵胶囊中芍药苷的含量

目的测定乙肝灵胶囊中芍药苷的含量。方法采用HPLC法,色谱柱采用Beckman C18反相柱。流动相:甲醇-0.05mol.L-1磷酸二氢钾溶液-醋酸-异丙醇(67∶173∶4∶4),流速为0.8ml.min-1,检测波长为240nm。结果本法线性关系良好(r=0.9995),平均加样回收率为98.44%,RSD=0.77%(n=6)。结论本法简便易行,结果准确,重现性好,可用于乙肝灵胶囊的质量控制。     

荧光分光光度法测定何首乌及人参首乌胶囊中总蒽醌的含量

目的:建立测定何首乌及人参首乌胶囊中总蒽醌含量的方法。方法:荧光分光光度法。以最佳 pH 条件的无水乙醇为溶剂,在λ_(EX)=440nm、λ_(EM)=515nm 处测定总蒽醌含量。结果:在0.03～0.15μg·mL~(-1)范围内,大黄素浓度和荧光强度有良好的线性关系,回归方程为 F=194.36C 2.9642,r=0.9996。平均回收率何首乌为98.1%,RSD 为1.9%;人参首乌胶囊为98.6%,RSD 为2.0%。测得总蒽醌含量何首乌中为0.522 mg·g~(-1),人参首乌胶囊中为0.443mg·g~(-1)。结论:本法简便快捷,准确灵敏,重复性好,可用于何首乌及人参首乌胶囊的质量控制。     

RP-HPLC法测定复方首乌合剂中大黄素的含量

目的:建立以反相高效液相色谱法测定复方首乌合剂中大黄素含量的方法。方法:色谱柱为Diamonsil C_(18)(150 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(68:32),检测波长为220 nm。结果:大黄素的检测浓度在7.8～78.0μg·mL~(-1)范围内与峰面积积分值呈良好线性关系(r=0.9998);平均回收率为98.25%,RSD=1.09%(n=9)。结论:本法准确、灵敏、重现性好,可用于复方首乌合剂的质量控制。     

HPLC法测定肝脂清胶囊中大黄素、大黄酚的含量

目的:建立肝脂清胶囊中大黄素、大黄酚的含量测定方法。方法:采用高效液相色谱法,以waters ODS C_(18)柱为固定相,甲醇-0.1%磷酸溶液(85:15)为流动相,检测波长254nm,流速1.0ml·min~(-1),柱温室温。结果:大黄素在13.84～83.04ng (r=0.9998),大黄酚在27.92～167.52ng(r=0.9998)范围内呈良好线性关系,平均回收率大黄素为99.47%、RSD为1.11%;大黄酚99.60%,RSD为1.09%。结论:本方法简便,准确,重现性好,为控制肝脂清胶囊的质量提供了科学依据。     

HPLC法测定复方五仁醇胶囊中五味子醇甲的含量

建立测定复方五仁醇胶囊中五味子醇甲含量的HPLC分析方法。采用DiamonsilTMC18色谱柱,甲醇-水(70∶30)为流动相,检测波长250nm。五味子醇甲在16.16～113.12μg·mL-1之间与峰面积呈良好的线性关系(r=0.9996,n=6),平均回收率98.08%,RSD=1.24%。本法操作简便、快速、准确,可用于复方五仁醇胶囊的含量测定。     

HPLC法同时测定复方苏润江滴丸中秋水仙碱、芦荟苷及芦荟大黄素的含量

目的:建立高效液相色谱法同时测定复方苏润江滴丸中秋水仙碱、芦荟苷、芦荟大黄素的含量。方法:采用Cosmosil-C18色谱柱(250 mm×4.6 mm,5μm),柱温为35℃,以甲醇(A)和水(B)为流动相,梯度洗脱[0～23 min,A-B(45∶55);23～40 min,A-B(65∶35)],流速1 mL·min-1,双波长检测:254 nm(检测芦荟大黄素),350 nm(检测秋水仙碱和芦荟苷)。结果:样品中秋水仙碱、芦荟苷和芦荟大黄素分离良好,秋水仙碱在16.54～82.71 mg·L-1(r=0.9998)、芦荟苷在13.19～105.54 mg·L-1(r=0.9997)、芦荟大黄素在6.00～47.97 mg·L-1(r=0.9999)范围内均呈良好线性关系;秋水仙碱、芦荟苷和芦荟大黄素的回收率分别为99.53%(RSD为1.3%),97.70%(RSD为1.0%),100.8%(RSD为0.96%),供试品溶液在12 h内稳定。结论:该方法简单准确,专属性强,重现性好,可用于同时测定复方苏润江滴丸中秋水仙碱、芦荟苷和芦荟大黄素的含量。     

HPLC法测定大黄通便颗粒中大黄素和大黄酚的含量

建立大黄通便颗粒中大黄素和大黄酚含量的HPLC测定方法.采用Spherixorb C18色谱柱,流动相:甲醇-0.1%磷酸溶液(90:10),流速:0.8ml·min-1,检测波长:254nm.线性范围:大黄素0.0135～0.2160μg(r=0.9998),大黄酚0.0240～0.3840μg(r=0.9995).平均加样回收率(n=5)分别为大黄素100.8%,RSD=1.1%;大黄酚100.2%,RSD=0.8%.本法简便,快速,结果准确.     

HPLC法测定肾衰宁胶囊中的4种成分

目的建立HPLC法同时测定肾衰宁胶囊中丹参素、原儿茶醛、丹酚酸B和大黄素的含量。方法采用Agilent Zorbax Eclipse XDB-C_(18)色谱柱(150 mm×4.6 mm,5μm);流动相为乙腈(A)-甲醇(B)-5 mL·L~(-1)磷酸溶液(C),梯度洗脱;流速:1.0 mL·min~(-1);柱温:30℃;丹参素、原儿茶醛和丹酚酸B的检测波长均为280 nm,大黄素的检测波长为254 nm。结果丹参素、原儿茶醛、丹酚酸B和大黄素分别在66.79～1 068.64 (r_1=0.999 6),5.63～90.15 (r_2=0.999 9),748.80～11 980.80 (r_3=0.999 8)和500.00～8 067.68μg·mL~(-1)(r_4=0.999 9)范围内呈良好的线性关系,平均回收率分别为98.24%(RSD=0.13%),98.55%(RSD=0.45%),98.37%(RSD=0.30%)和99.44%(RSD=0.41%)。结论该方法分离效果好、简便、重复性好,适用于肾衰宁胶囊的质量控制。     

肝炎康胶囊质量标准的建立

目的:研究肝炎康胶囊的质量标准。方法:分别采用薄层色谱法鉴别肝炎康胶囊中的虎杖、黄芪、太子参、半枝莲、白花蛇舌草、丹参、柴胡;用高效液相色谱法测定肝炎康中的大黄素含量。结果:薄层色谱法能明显从肝炎康胶囊中鉴别出虎杖、黄芪、太子参、半枝莲、白花蛇舌草、丹参、柴胡。测得肝炎康胶囊中所含大黄素的含量是2.05 mg·g-1,大黄素的含量在范围2.34~74.88μg·ml-1之间呈现良好的线性关系(r=0.999 4),平均回收率为100.5%,RSD为1.52%(n=9)。结论:肝炎康胶囊质量标准准确、可靠,可作为肝炎康胶囊的质量控制方法。     

反相HPLC法测定六味安消胶囊及大黄药材中大黄素的含量

目的:用反相HPLC法测定六味安消胶囊及大黄药材中大黄素的含量.方法:采用CLC-ODS C18色谱柱(5μm,4.6×150mm),流动相:甲醇-0.4%磷酸溶液(85∶15),检测波长:438nm,流速:1.2ml/min,柱温25℃.结果:大黄素的平均回收率为98.56%(RSD=2.61%,n=12),线性范围为0.0798～0.638μg(r=0.9999).结论:本法快速,准确,灵敏,简便易行.     

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.