HPLC-ELSD法同时测定新氢化可的松乳膏中硫酸新霉素和氢化可的松的含量

目的建立HPLC-蒸发光散射检测器(ELSD)法,同时测定新氢化可的松乳膏中硫酸新霉素和氢化可的松的含量。方法色谱条件:C18色谱柱(150 mm×4.6 mm,5μm);流动相:乙腈-0.1 mol/L三氟乙酸溶液(梯度洗脱);漂移管温度:110℃;载气流速:2.6 L/min。用硫酸新霉素和氢化可的松对照品分别测定新氢化可的松乳膏中硫酸新霉素和氢化可的松的含量。结果硫酸新霉素进样量在0.7～4.3μg范围内(r=0.999 7),氢化可的松进样量在1.0～2.9μg范围内(r=0.999 9)。结论该方法快速、简便、重现性好,灵敏度高。     

HPLC-CAD法测定硫酸新霉素中新霉素B、新霉素C、新霉胺及其他有关物质

目的 建立测定硫酸新霉素中新霉素B、新霉素C、新霉胺及其他有关物质的高效液相色谱-电喷雾检测器(HPLC-CAD)方法。方法 采用Waters HSS T3色谱柱(4.6mm×250mm, 5μm)，以0.15mol/L三氟乙酸水溶液为流动相，流速1.0mL/min，柱温30℃，电喷雾检测器的雾化温度为45℃。结果 新建方法对新霉素B、新霉素C、其他有关物质分离度良好，精密度、重复性和回收率均满足分析要求。新霉素B、新霉胺浓度与峰面积线性关系良好(r＞0.995)，检出限可达到0.02μg和0.003μg。结论 新建方法分离度好、灵敏度高，可以检出更多的杂质，可以满足硫酸新霉素原料有关物质分析的要求。     

高效液相色谱法测定盐酸溴己新及其片剂的含量和有关物质

目的:建立高效液相色谱法测定盐酸溴己新及其片剂的含量和有关物质。方法:采用 C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为醋酸溶液(pH 3.4)-甲醇(30∶70),流速1.0 mL·min~(-1),检测波长254 nm。结果:盐酸溴己新在18.70～130.90μg·mL~(-1)范围内,线性关系良好,回归方程 Y=30.1549 X 5.4729,r=0.9999。平均回收率为98.24%(n=9)。最低检出限为0.086μg·mL~(-1)。结论:本法快速、简便、准确,专属性强。     

HPLC-ELSD法定量检测硫酸新霉素中新霉胺

目的建立测定硫酸新霉素中有关物质新霉胺的HPLC ELSD法。方法色谱柱Zorbax SB C18（4.6 mm×250 mm,5 μm）,柱温：25 ℃;流动相：甲醇：0.1 mol•mL 1三氟乙酸溶液 （8：92）;流速0.8 mL•min 1;漂移管温度：55 ℃;载气压力：3.6 MPa;Gain：6。结果新霉胺最低检测限为40 ng,最低定量限为80 ng,在0.08～1.60 μg范围内呈很好的线性关系,r＝0. 999 6,平均回收率97.3%,RSD＝2.6%（n＝9）。结论该方法准确、专属性强,可用于硫酸新霉素中有关物质新霉胺的含量测定。     

HPLC法测定蒿甲醚注射液的含量

目的:建立蒿甲醚注射液含量测定的高效液相色谱方法。方法:采用 Alltima C_(18)柱(150 mm×4.6 mm,5μm),以乙腈-水(70:30)为流动相,流速为1.0 mL·min~(-1),外标法测定,检测波长为210 nm。结果:线性范围为190～3800μg·mL~(-1),r=0.9999;平均回收率(n=3)分别为99.2%(RSD=0.68%),99.6%(RSD=0.55%),99.6%(RSD=0.18%);最低检测限为1.14μg;最低定量限为3.05μg。结论:该法准确、简便,适用于蒿甲醚注射液的含量测定。     

HPLC-ELSD法测定1，4-丁二磺酸腺苷蛋氨酸中1，4-丁二磺酸阴离子的含量

目的:建立1,4-丁二磺酸腺苷蛋氨酸中1,4-丁二磺酸阴离子含量的测定方法。方法:采用高效液相-蒸发光散射检测方法。色谱柱:Supelcosil LC—SCX(250 mm×4.6 mm,5μm),流动相:0.5 mol·L~(-1)甲酸铵溶液(pH 2.8),流速:0.4 mL·min~(-1);ELSD 漂移管温度:105℃,载气流速:3.5 L·min~(-1)。结果:最低检测限为0.8μg;最低定量限为1.6μg;线性范围为2.1～21.5μg(r=0.9999);平均加样回收率为98.5%,RSD=2.2%(n=9)。结论:该方法简便、快速,结果准确,重现性好。     

HPLC-ELSD测定硫酸庆大霉素注射液含量及其有关物质的研究

目的 研究不同操作模式的蒸发光散射检测器和不同的对照品随行曲线对庆大霉素含量及有关物质测定的影响.方法 色谱柱为Phenomex Gemini C_(18)和Agilent Zorbax C_(18)(250 mm×4.6 mm,5 μm);流动相为0.2 mol·L~(-1)三氟乙酸溶液-甲醇(94:6)、(96:4);流速0.6 mL·min~(-1);柱温30℃;蒸发光散射检测器Waters 2424的飘移管温度为65℃,气体流速为20 psi;蒸发光散射检测器Alltech2000的飘移管温度为110℃;气体流速2.8 L·min~(-1);进样量20μL.结果 对庆大霉素组份测定结果均无显著影响,对有关物质测定结果有影响.结论 庆大霉素组分测定可不采用对照品随行标准曲线法及浓度与峰面积的双对数回归方程进行计算,而直接进行峰面积归一化法进行组分含量计算,大大简化了操作与计算.有关物质不宜采用峰面积归～化法计算杂质的量,应采用对照品随行标准曲线法及浓度与峰面积的双对数回归方程进行计算.     

高效液相色谱法测定烯丙雌醇的含量及有关物质

目的:建立烯丙雌醇含量测定及有关物质检查方法。方法:采用反相高效液相色谱法。色谱柱:Alltima C_(18)柱(5μm,4.6 mm×150 mm),流动相:乙睛-水(95:5),检测波长:205 nm(含量测定),210 nm(有关物质),流速:1.0 mL·min~(-1)。结果:烯丙雌醇与各主要杂质及强制破坏产生的降解产物的杂质峰均分离良好,烯丙雌醇浓度在107.2～964.8μg·mL~(-1)范围内,与峰面积呈良好的线性关系,回归方程:A=11370C 40119,r=0.9998(n=7);精密度为0.34%(n=6);平均回收率为99.76%(RSD=0.64%,n=9),最低检出限为4.08 ng。结论:该法准确、灵敏、专属件强,可用于烯丙雌醇的含量测定利有关物质检查。     

反相高效液相色谱法测定阿德福韦酯的含量及其有关物质

目的:建立反相高效液相色谱法测定阿德福韦酯含量及其有关物质。方法:采用 Inertsil C_8硅烷键合硅胶为填料的色谱柱(250 mm×4.6 mm,5 μm);以乙腈-25 mmol·L~(-1)磷酸二氢钾溶液(pH 6.0)(40:60)为流动相,流速1.0 mL·min~(-1),检测波长为262 nm。结果:杂质及降解产物能与阿德福韦酯基线分离;浓度存10.28～154.20μg·mL~(-1)范围内与峰面积呈良好线性关系,r=1.0000(n=8);最低柃测限为0.04 ng。结论:本法准确、简便,适用于阿德福韦酯及其有关物质的含量测定。     

HPLC法测定注射用头孢尼西钠含量及有关物质

目的:用 HPLC 法测定注射用头孢尼西钠的含量及其有关物质。方法:采用 Kromasil C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-水-0.2 mol·mL~(-1)磷酸二氢铵(21:74:5)为流动相,流速1.0 mL·min~(-1),检测波长为254 nm;柱温:40℃。结果:头孢尼西钠与其相邻杂质峰能完全分离,头孢尼西钠在22～132μg·mL~(-1)浓度范围内线性关系良好(r=0.9999)。结论:该法简便、准确、专属性好,可以用于注射用头孢尼西钠的含量测定及有关物质检查。     

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.