HPLC法测定益母草颗粒中水苏碱的含量

目的建立高效液相色谱法测定益母草颗粒中水苏碱含量的方法。方法采用YWG-C18柱,以0.1mol·L-1磷酸盐溶液(pH5.5)为流动相,检测浓度192nm,流速0.8mL·min-1柱温30℃。结果水苏碱在0.5～4.0μg范围内线性关系良好,平均回收率为96.70%,RSD=0.71%,r=0.9998(n=6)。结论本方法操作简便,准确稳定,可作为测定益母草颗粒中水苏碱的定量分析。     

中药材益母草中水苏碱含量鉴定分析

目的 研究中药材益母草的水苏碱成分的含量鉴定.方法 应用高效液相色谱法测定中药材益母草中水苏碱成分的含量,以Kromasil KR60-5CN为色谱柱,乙腈-甲醇溶液为流动相,以外标法进行检测,设定柱温32℃,流速1.5 ml/min,检测波长210 nm.结果 水苏碱回归方程为Y=1206.578X-173.562,水苏碱进样量在1.00～25.00 μg范围内具有良好的线性关系,r=0.9954,样品平均加样回收率为98.83% (n=9),RSD为0.95%.结论 用高效液相色谱法测定中药材益母草中水苏碱含量准确县可靠,可重复利用,是控制该制剂质量的有效方法.     

HPLC法测定不同产地益母草中盐酸水苏碱的含量

目的:建立改性活性炭-中性氧化铝纯化方法,用HPLC法测定不同产地益母草中盐酸水苏碱的含量.方法:用三乙胺处理活性炭,制备载氮改性活性炭,益母草经乙醇提取后过改性活性炭-中性氧化铝柱,系统考察活性炭改性方式、用量、中性氧化铝用量、上样及洗脱流速、乙醇洗脱体积;采用-NH2柱在反相条件下测定不同产地益母草中盐酸水苏碱的含量.结果:在选定的色谱条件下盐酸水苏碱可以得到较好的分离,线性范围2.046～20.46μg,平均回收率为98.31％,RSD为1.434 1％(n=6).11个产地的益母草药材中盐酸水苏碱含量差异较大.结论:该方法测定准确、稳定、重复性好,可用于不同产地益母草药材及饮片的质量评价.     

花期对益母草药材中盐酸水苏碱和盐酸益母草碱含量的影响

摘 要: 目的 研究开花对益母草药材中盐酸水苏碱含量的影响。方法 在同一地区不同时期采收益母草药材样品;运用药典法水苏碱进行测定。 结果 开花过程中益母草药材中盐酸水苏碱的含量不断降低。 结论 开花对益母草药材中盐酸水苏碱含量影响较大。     

HPLC法测定益母草膏中盐酸水苏碱的含量

目的建立高效液相色谱法测定益母草膏中盐酸水苏碱的含量测定方法。方法采用甲醇溶解样品并去除样品中糖分等杂质的方法制备供试品溶液,CAPCELL Pak C18柱(5μm,150mm×4.6mm)为分析柱;甲醇-0.05mol·L-1磷酸二氢钾溶液(67∶33)[1]为流动相;紫外检测波长为215nm;柱温为30℃;流速为1.0mL·min-1;按外标法计算结果。结果盐酸水苏碱进样量在2.05～12.30μg范围内与峰面积呈良好的线性关系,r=0.9999,样品平均加样回收率为98.9%,RSD为0.4%;重复性实验RSD为0.4%。结论方法简便、准确,重现性好,可作为益母草膏的质量控制。     

HPLC-ELSD测定益母草颗粒中盐酸水苏碱的含量

目的建立HPLC-ELSD测定益母草颗粒中盐酸水苏碱的含量。方法色谱柱为Venusil HILIC丙基酰胺键合硅胶柱(250 mm×4.6 mm,5μm);柱温为25℃;流动相为乙腈-0.2%冰醋酸溶液(80∶20);流速为0.8 mL.min 1;进样量为10μL;漂移管温度为80℃,氮气流速为1 L.min-1。结果盐酸水苏碱在0.646 5~12.93μg内呈良好的线性关系,r=0.999 4(n=5);平均加样回收率为98.48%,RSD=1.15%(n=9)。结论该方法简便、快速、准确、重复性和稳定性好,可作为益母草颗粒的盐酸水苏碱含量测定方法。     

RP-HPLC测定产妇安口服液中水苏碱的含量

目的　建立RP -HPLC测定产妇安口服液中益母草有效成分之一的水苏碱。方法　采用Kromasil-NH2 色谱柱 (2 5 0mm× 4.6mm ,5 μm) ,乙腈 -水 (80∶2 0 )为流动相 ,流速 1.0ml·min-1。样品加入新配制的 2 %雷氏盐沉淀后 ,丙酮溶解 ,再用硫酸银与氯化钡溶液将水苏碱游离出来 ,定容后离心 ,取上清液 10 μl进样 ,2 10nm检测 ,按外标法定量。结果　标准曲线线性范围为 0 .0 5～ 0 .4g·L-1,日内RSD <4%,方法回收率在 97%～ 10 5 %之间。结论　所用方法简便 ,测定结果准确可靠。     

HPLC法测定复方杜仲丸中盐酸水苏碱与黄芩苷的含量

目的： 建立HPLC法测定复方杜仲丸中盐酸水苏碱与黄芩苷的含量。方法：采用高效液相色谱（HPLC）法,强阳离子交换(SCX)色谱柱测定盐酸水苏碱的含量,十八烷基硅烷键合硅胶测定黄芩苷的含量。结果：盐酸水苏碱在0.01012～1.012 mg?mL-1、黄芩苷在0.00501～0.501 mg?mL-1浓度与峰面积具有良好的线性关系（r值均为0.9998）;盐酸水苏碱与黄芩苷回收率均符合要求。结论：该方法可控制复方杜仲丸中益母草与黄芩的含量。     

亲水作用色谱-蒸发光散射法测定益母草中盐酸水苏碱的含量

目的:建立亲水作用色谱-蒸发光散射检测器联用测定益母草中盐酸水苏碱含量的方法。方法:采用HILIC柱(250mm×4.6 mm,5μm);乙腈-0.2%冰醋酸溶液(80∶20)为流动相;Alltech2000蒸发光散射检测器:漂移管温度80℃,气体流速2.0 L.min-1;流速0.5 mL.min-1。结果:盐酸水苏碱进样量在0.536～10.713μg范围内呈良好的线性关系,平均回收率为101.9%,RSD为1.4%。结论:此方法简便、灵敏度高,重现性好,可用于益母草的含量测定。     

RP-HPLC法测定贵州、湖南卷柏中穗花杉双黄酮的含量

目的:建立以反相高效液相色谱法测定贵州、湖南卷柏中穗花杉双黄酮含量的方法。方法:色谱柱为Purospher star RP-C18(250mm×4·6mm,5μm),流动相为甲醇-0·1%磷酸溶液(65∶35),流速为0·8mL·min-1,检测波长为337nm,柱温为25℃。结果:贵州、湖南卷柏药材中的穗花杉双黄酮的含量分别为0·19%、0·51%。结论:本方法灵敏、准确,可为选择卷柏道地药材提供依据。     

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.