HPLC法测定苦参总碱中苦参碱与氧化苦参碱的含量

目的:采用高效液相色谱法测定苦参总碱中苦参碱和氧化苦参碱的含量。方法:采用 Elite Hypersil NH_2柱(5μm,250mm×4.6 mm),乙腈-无水乙醇-3%磷酸溶液(81:10:9)为流动相,流速:1.0 mL·min~(-1),检测波长220 nm,柱温:25℃,进样量:10 μL。结果:苦参碱、氧化苦参碱的线性范围分别为5.32～53.2μg·mL~(-1)(r=0.9997),65.7～525.6μg·mL~(-1)(r=0.9995)。苦参碱平均加样回收率为99.5%,RSD=1.0%(n=6);氧化苦参碱的平均加样回收率为99.7%,RSD=0.6%(n=6)。结论:本方法操作简便、快速、可靠,可用于控制苦参总碱质量。     

心律宁片中苦参碱和氧化苦参碱的含量测定

目的:建立心律宁片中苦参碱和氧化苦参碱含量的测定方法。方法:色谱柱为Alltima Amino(250mm×4.6mm,5μm),流动相为乙腈-无水乙醇-3%磷酸溶液(80:10:10),检测波长为220nm,流速为1.0ml·min~(-1);柱温:室温。结果:苦参碱线性范围是0.168μg～3.360μg,r=0.999 7,氧化苦参碱线性范围是0.124μg～2.480μg,r=0.999 3,苦参碱及氧化苦参碱的平均回收率分别为101.1%(RSD=1.22%)和100.2%(RSD=1.91%)(n=6)。结论:方法快速简便,重复性良好,可用于测定心律宁片中苦参碱和氧化苦参碱的含量。     

RP-HPLC测定苦参素注射液中氧化苦参碱的含量

目的:建立测定苦参素注射液中氧化苦生碱含量的方法。方法:色谱柱为Phenomsil-C_(18)柱(250 mm×4.6 mm,5μm),流动相为0.05 mol·L~(-1)磷酸二氢钾溶液-乙腈(92:8),检测波长220 nm,流速1.0 ml·min(-1)。结果:氧化苦参碱的线性范围为50～400μg·ml~(-1)(r=0.999 9)平均回收率为98.65%,RSD=1.50%。结论:该法简便,快速,准确。     

RP—HPLC法测定苦参素胶囊的含量和有关物质

目的:建立高效液相色谱法测定苦参素胶囊中氧化苦参碱的含量和有关物质的量。方法:采用 C_(18)色谱柱(250 mm×4.0 mm,5μm);以0.05 mol·L~(-1)磷酸二氢钾溶液(用磷酸调 pH 至3.5)-甲醇(83:17)为流动相,流速:1.0 mL·min~(-1),检测波长215 nm。结果:在建立的色谱条件下,氧化苦参碱与杂质能完全分离。氧化苦参碱线性范围为40.0～200μg·mL~(-1)(r=0.9999)。结论:所用方法简便、准确,专属性好。     

离子对RP-HPLC同时测定复方苦参注射液中氧化苦参碱、槐果碱和苦参碱的含量

目的:建立同时测定复方苦参注射液中氧化苦参碱、槐果碱和苦参碱含量的方法。方法:采用离子对RP-HPLC法,色谱柱为Diamonsi C18(2)(250 mm×4.6 mm,5μm),流动相为乙腈-甲醇-水(35∶10∶55,水相中含5.5%磷酸和1.5%SDS),流速1.0 mL.min-1,检测波长220 nm,柱温为室温。结果:氧化苦参碱、槐果碱和苦参碱分别在9.92～99.2μg.mL-1(r=0.9991,n=5)、4.08～32.64μg.mL-1(r=0.9993,n=5)和20.16～161.28μg.mL-1(r=0.9996,n=5)范围内呈良好线性关系;平均回收率(n=6)分别为98.9%(RSD=1.2%),99.5%(RSD=1.4%)和100.2%(RSD=1.0%)。结论:本文建立的测定方法可应用于复方苦参注射液质量评价。     

RP—HPLC法测定田基黄中异巴西红厚壳素的含量

目的:建立测定田基黄中异巴西红厚壳素含量的方法。方法:采用 RP-HPLC 法,色谱柱为 Diamonsil C_(18)(200 mm×4.6 mm,5 μm);以乙腈-甲醇-水-磷酸(45:15:50:0.05)为流动相;流速为1.0 mL·min~(-1);柱温为室温;检测波长为254 nm。结果:异巴西红厚壳素浓度在5.01～80.2 μg·mL~(-1)范围内与峰面积呈良好线性关系,r=0.9999(n=5);平均回收率为97.5%(n=9)。结论:本方法简便、快速、准确,可用于田基黄中异巴西红厚壳素的含量测定。     

HPLC法测定止痢宁片中苦参碱与氧化苦参碱的含量

采用高效液相法同时测定止痢宁片中苦参碱和氧化苦参碱的含量.以Allttima Amino 100A为色谱柱,流动相乙腈-无水乙醇-3%磷酸(781111),流速0.8mL·min-1,检测波长220nm.苦参碱的线性范围0.493～1.479μg,r=0.9997;氧化苦参碱的线性范围0.2054～0.7512μg,r=0.9994.平均加样回收率苦参碱为96.53%,RSD=1.83%;氧化苦参碱为95.02%,RSD=1.96%.本方法简便,专属,精密度好,分离效果好.     

HPLC法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量

目的:采用高效液相色谱法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量。方法:采用 Li-chrospher C_(18)(5 μm,4.6 mm×250 mm)色谱柱,以甲醇-水-冰醋酸(40:60:0.3)为流动相,流速1.0 mL·min~(-1),检测波长272 nm,柱温35℃。结果:对乙酰氨基酚线性范围为19.93～199.32μg·mL~(-1)(r=0.9998),平均回收率(n=9)为99.2%;乙酰水杨酸线性范围为36.00～359.96μg·mL~(-1)(r=0.9999),平均同收率(n=9)为99.7%;咖啡因线性范围为4.90～49.04μg·mL~(-1)(r=0.9998),平均同收率(n=9)为98.8%。结论:方法简使,结果准确,适用于该产品的质量控制。     

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。     

高效液相色谱法测定复方苦参素胶囊中苦参碱的含量

目的:建立高效液相色谱法测定复方苦参素胶囊中苦参碱的含量。方法:以 Hypersil C_8色谱柱(4.6mm×150mm,5μm)为色谱柱,柱温25℃,用甲醇-水-三乙胺(45:55:0.02)为流动相,流速0.8mL·min~(-1)。进样量10μL,于220nm 波长处,以外标法测定。结果:苦参碱在10.7～161.0μg·mL~(-1)浓度范围内线性关系良好(r=0.9999)。平均回收率为99.6%。结论:本方法灵敏、简便、准确。     

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.