RP-HPLC测定鸡骨草中的下箴刺桐碱

目的建立测定鸡骨草药材中下箴刺桐碱的方法。方法采用RP-HPLC法,色谱柱为Lichrospher C18(250 mm×4.6mm,5μm),流动相为水-甲醇-乙腈-冰醋酸-三乙胺(82:13:5:0.2:0.3),流速为1.0 ml.min-1,检测波长为220 nm,柱温为室温。结果线性范围2.9-17.4 mg.L-1(r=0.9999,n=6);平均回收率为102.9%,RSD=1.9%(n=6)。结论所建方法简便、快速,结果准确,可为鸡骨草药材的质量评价提供参考。     

鸡骨草药材指纹图谱研究

目的 建立鸡骨草药材的指纹图谱.方法 采用RP-HPLC高效液相色谱法,Phenomenex-ODS色谱柱(250 mm ×4.0 mm,5μm),甲醇-0.5%冰醋酸溶液,梯度洗脱,流速1.0 ml/min,检测波长270 nm.结果 建立了鸡骨草药材指纹图谱共有模式,显示5个共有峰,指认了相思子碱1个特征峰.结论 ...     

牛大力中刺桐碱的分离鉴定和含量测定

目的:首次从牛大力药材中分离制备刺桐碱对照品并应用高效液相色谱方法建立牛大力药材中刺桐碱含量的测定方法。方法:Agilent(SB-C18)(5μm,4.6 mm×150 mm)色谱柱,乙腈-水(1∶9)为流动相,流速为0.8 mL.min-1,检测波长为280 nm,柱温30℃。结果:刺桐碱在0.0113~2.825 mg.mL-1范围内呈良好的线性关系(r=0.9996,n=5),平均回收率(n=9)为99.6%。结论:本方法准确,简便,重复性好,可用于牛大力药材中刺桐碱的含量测定。     

鸡骨草药材指纹图谱研究

目的建立鸡骨草药材的指纹图谱。方法采用RP-HPLC高效液相色谱法,Phenomenex-ODS色谱柱(250 mm×4.0 mm,5μm),甲醇-0.5%冰醋酸溶液,梯度洗脱,流速1.0 ml/min,检测波长270 nm。结果建立了鸡骨草药材指纹图谱共有模式,显示5个共有峰,指认了相思子碱1个特征峰。结论 HPLC指纹图谱中各峰分离度较好,方法具有较好的精密度、重现性和稳定性,符合指纹图谱的要求,可用于鸡骨草药材质量控制。     

HPLC法同时测定泌感颗粒中小檗碱和槲皮素的含量

目的:建立同时测定泌感颗粒中小檗碱和槲皮素含量的方法。方法:采用高效液相色谱法,色谱柱为 Diamonsil C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾溶液(27:73),流速为1.0 mL·min~(-1),检测波长为360nm。结果:小檗碱浓度在8.33～41.6μg·mL~(-1)范围内线性关系良好(r=0.9997),平均方法回收率(n=6)为98.6%;槲皮素浓度在4.08～20.4μg·mL~(-1)范围内线性关系良好(r=0.9998),平均方法回收率(n=6)为97.8%;结论:本法简便,准确度和重复性好,可用于泌感颗粒中小檗碱和槲皮素的同时测定。     

相思子质量标准改进

摘要 目的：提高相思子质量标准。方法：显微鉴定相思子组织特征;采用薄层色谱法对相思子及主要成分相思子碱进行定性鉴别;采用高效液相色谱法测定相思子碱的含量。结果：栅状细胞、子叶细胞、支持细胞特征明显;薄层色谱斑点清晰,专属性强;相思子碱在0.1μg-4μg范围内线性关系良好(r=1),平均回收率为99.5%,RSD为0.75%（n=6）。结论：本方法操作简便,专属性强,重复性好,可作为相思子的质量控制方法。     

HPLC法测定吴茱萸超微速溶饮片中吴茱萸碱、吴茱萸次碱及柠檬苦素的含量

目的建立一种同步测定吴茱萸超微速溶饮片中吴茱萸碱,吴茱萸次碱及柠檬苦素含量的高效液相色谱方法。方法采用Hypersil ODS2C18柱(4.6mm×250mm,5μm),岛津LC-20AD高效液相色谱仪,流动相为乙腈-水-四氢呋喃-冰醋酸(34:64.7:1.1:0.2),流速:1.0mL/min,检测波长:225nm,柱温:30℃。结果吴茱萸碱、吴茱萸次碱、柠檬苦素进样量分别在0.1016～2.032μg(r2=0.9999,n=6)、0.0974～1.948μg(r2=0.9999,n=6)、0.7010～14.02μg(r2=0.9999,n=6)范围内与峰面积呈良好线性关系,平均回收率分别为100.37%(RSD=1.29%,n=6)、99.11%(RSD=0.83%,n=6)、99.30%(RSD=0.52%,n=6)。结论该测定方法简便,测定结果准确,重复性好,可作为质量控制方法。     

HPLC测定风湿安泰片中马钱子碱和士的宁的含量

目的:采用反相高效液相色谱法测定风湿安泰片中士的宁和马钱子碱的含量。方法:采用 Hypersil BDS C_(18)色谱柱(4.6 mm×250 mm,5 μm),保护柱(4.6 mm×12 mm);乙腈-0.3%三乙胺溶液(磷酸调 pH=2.6)(10:90)为流动相,流速:1.0 mL·min~(-1),柱温:室温,检测波长:254 nm。结果:士的宁在4.6～46μg·mL~(-1)(r=0.9998),马钱子碱在2.65～26.5μg·mL~(-1)(r=0.9998)范围内呈良好的线性关系,士的宁的平均回收率(n=5)为101.1%,RSD 为2.8%;马钱子碱的平均回收率(n=5)为99.6%,RSD 为2.9%。结论:本方法准确、简便、快速,适用于风湿安泰片的质量控制。     

RP—HPLC法测定白头翁中23-羟基白桦酸的含量

目的:建立中药白头翁药材中23-羟基白桦酸的 RP-HPLC 含量测定方法。考察了5个地区的商品药材中23-羟基白桦酸的含量。方法:高效液相色谱法,色谱柱为 Agilent Zorbax SB-C_(18)(250 mm×4.60 mm,5μm),流动相:乙腈-0.2%醋酸水溶液(62∶38),流速为0.8 mL·min~(-1),分析时间20 min;检测波长204 nm,进样体积为20μL。结果:23-羟基白桦酸进样量与峰面积呈良好线性关系,线性范围为0.20～4.0μg,r=0.9999(n=5);回收率为97.4%～104.7%(n=9)。结论:本方法首次测定了5个地区白头翁药材中23-羟基白桦酸的含量,该方法快速、简便,重复性好。     

RP-HPLC法测定北豆根药材中5个生物碱的含量

目的:采用RP-HPLC法同时测定中药材北豆根中青藤碱、蝙蝠葛苏林碱、蝙蝠葛诺林碱、蝙蝠葛新诺林碱和蝙蝠葛碱5种生物碱的含量。方法:采用色谱柱Welchrom-C18(250 mm×4.6 nm,5 mm),以甲醇(A)-乙腈(B)-0.4%二乙胺水溶液(C)为流动相,梯度洗脱[0～13 min,A-B-C(18:20:62);13～45 min,A-B-C(18:20:62)→A-B-C(37:20:43);45～60min,A-B-C(37:20:43)];流速1.0 mL·min-1;检测波长为285 nm。结果:青藤碱、蝙蝠葛苏林碱、蝙蝠葛诺林碱、蝙蝠葛新诺林碱和蝙蝠葛碱5种生物碱的线性范围分别为0.016～0.2μg(r=0.9995),0.029～0.363μg·mL-1(r=0.9996),0.09～1.125μg·mL-1(r=0.9996),0.336～4.2μg·mL-1(r=0.9997)与0.172～2.15μg·mL-1(r=0.9996);加样同收率(n=6)分别为99.2%,98.5%,102.2%,96.5%和98.4%。结论:该方法简便、快速、准确,重复性好,可以用于北豆根药材及其制剂的含量测定。     

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.