柱层析法纯化灯盏乙素的研究

目的优选灯盏乙素的柱层析纯化条件。方法采用高效液相色谱法检测纯度,考察了不同固定相和流动相对灯盏乙素分离效果的影响。结果灯盏乙素的最佳纯化工艺条件为:固定相200-300目的硅胶柱,流动相V(CH2Cl2)∶V(CH3OH)=5∶1,常压洗脱。结论该方法操作简单,分离效果好,使用成本低。     

正交函数分光光度法测定芫花根注射液中二萜原酸酯类的含量

芫花根注射液是一种粗制剂,成分复杂,含量测定困难,其主要引产成分为芜花酯甲,芫花酯乙,芫花酯丙和芜花酯丁等瑞香烷型二萜原酸酯类,其中以芫花酯甲含量最高。本文以芫花酯甲为标准品,用正交函数分光光度法,测定芫花根注射液中总瑞香烷型二萜原酸酯的含量。其平均回收率为98.9%,变异系数1.6%(n=9)。     

HPLC柱切换法对炔诺酮α,β-聚(3-羟丙基)-DL-天冬酰胺在兔体内释放炔诺酮的测定

以柱切换HPLC(CSHPLC)技术,对炔诺酮α,β-聚(3-羟丙基)-DL-天冬酰胺在家兔体内释放液中炔诺酮的血药浓度进行了测定,以自制ODS预柱,水为流动相联机净化、富集样品;以Shim-packCLC-ODS为分析柱,甲醇-水(7:3)为流动相。结果表明CSHPLC对炔诺酮血药浓度有良好的选择性,回收率为82.6%(n=5),日内和日间精密度(RSD)分别小于4%和6%。在血清0.22～1.10μg/m1范围内炔诺酮色谱峰面积与浓度有较好的线性关系(n=5,r=0.998).     

A rapid reversed phase high performance liquid chromatographic method for the determination of docetaxel (Taxotere®) in human plasma using a column switching technique

A rapid, simple and sensitive isocratic high performance liquid chromatography (HPLC) method was developed to measure the concentration of docetaxel in plasma samples with UV detection at 227 nm. The method uses a column switching technique with an Ultrasphere C₁₈ column (75×4.6 mm ID, 3μ, Altex, USA) as clean-up column and a CSC-nucleosil C₈ column (150×4.6 mm ID, 5μ, CSC, Montreal, Canada) as the analytical column. The mobile phase consisted of Phosphate buffer (30 mM, pH=3)-acetonitrile (47:53, v/v) with the flow rates of 1.1 and 1.3 ml min⁻¹ for clean-up and analytical columns, respectively. Paclitaxel was used as an internal standard. The plasma samples were extracted using a solid phase extraction method with Ammonium acetate (30 mM, pH=5)-acetonitrile (50:50, v/v) as final eluent. The extraction method showed a recovery of 92% for docetaxel. In this system, the retention times of docetaxel and Paclitaxel were 7.2 and 8.5 min, respectively. The detection limit of docetaxel in plasma is 2.5 ng ml⁻¹. This analytical method has a very good reproducibility (7.2% between-day variability at a concentration of 10 ng ml⁻¹). It is applicable in clinical and pharmacokinetic studies.     

薄层扫描法测定回生口服液中水苏碱的含量

采用醇沉及两次柱色柱的方法预处理样品，用薄层扫描法测定了样品水中苏碱的含量。λｓ＝４１５ｎｍ，λＲ＝５５０ｎｍ。测定结果表明，水苏碱含量与峰面积积分值线性范围为２。６￣８．３μｇ，ｒ＝０．９９８６，平均回收率为９７．４％，ＲＳＤ＝２．３％（ｎ＝６）。为回生口服液中水苏碱的含量测定提供了准确可靠的方法。     

柱分配色谱—紫外分光光度法检查测定乙酰水杨酸片

本文采用美国药典（ＸⅫ）柱分配色谱—紫外分光光度法检查ＡＳＡ片剂中的ＳＡ的限量，测定ＡＳＡ含量。比较不同操作时间对检查测定结果的影响。同中国药典（１９９０年版）方法比较。实验结果表明用ＵＳＰ（ⅩⅫ）方法检查测定ＡＳＡ的限量全过程在１小时内完成，结果准确，可排除干扰，重现性好。     

HPLC柱切换法测定血浆和尿样中头孢克肟浓度

用双泵HPLC柱切换系统直接进样测定血浆和尿样中头孢克肟(cefixime,CFIX)的浓度。血浆和尿样的回收率分别为99.1%和98.6%;最低检测浓度分别为0.05和0.2μg/ml;日内和日间的RSD小于5%;血浆和尿样浓度分别在0.1～3.2和1.0～32μg/ml范围内呈线性相关。此方法集样品净化、富集成分和色谱分析一次连续进行,操作简便、快速,可以进较大的样品量,灵敏度相对明显提高。     

用离子交换树脂柱式法光度测定血液中盐酸氯丙嗪

氯丙嗪是治疗精神病最有效的药物之一.近年来建立了高效液相色谱法和放射免疫法等较灵敏方法,但前者所用的仪器价格昂贵,不易普及推广.Forrest用离子交换树脂静态加热过滤处理的方法测定尿中氯丙嗪,简便易行,但空白值高,重复性较差.经作者将其改进成柱式法后,然后进     

Determination of Lansoprazole by Direct Injection of Plasma and High Performance Liquid Chromatography with Column Switching

建立了用柱切换测定血浆中兰索拉唑的方法。血样用蒸馏水简单稀释后注入填充ＬｉＣｈｒｏｍｐｒｅｐＲＰ２（２５～４０μｍ）的预柱上。用蒸馏水冲洗出血浆中蛋白质和其它极性成分。切换后，浓缩在预柱上的兰索拉唑被流动相甲醇０２ｍｏｌ·Ｌ１醋酸铵（６５：３５）反冲到分析柱ＳｈｉｍｐａｃｋＣＬＣＯＤＳ上进行分析。预柱用净化液进行消除和再生。本法有很好的精密度和回收率，检测限为０００５ｍｇ·Ｌ１，日内和日间测定相对标准差小于２５％和５３％。此分析方法已成功地用于测定自愿受试者的兰索拉唑药代动力学     

Design features of haemoperfusion columns containing activated charcoal

The performance of four haemoperfusion columns, containing polymer-coated activated charcoal, for removal of paracetamol, acetyl salicylic acid and sodium amylobarbitone has been examined. Dye-tracer studies were used to measure mean residence times, dispersion coefficients and dead volumes of the columns. The mass-transfer coefficients for the removal of these substances from blood were measured to define the importance of the boundary layer in determining the kinetics of extraction. Diffusion through this layer was found to be the rate-limiting step for paracetamol adsorption, but other factors also were found to be of importance for the other two substances. The results suggest that an efficient perfusion column would consist of a long, thin configuration rather than a squat, short shape.