薄层色谱溶剂系统的最优化方法——Ⅵ.均匀设计法的再探讨

就第Ⅱ报及第Ⅴ报提出的用于选取薄层色谱最佳溶剂系统的均匀设计法进行了进一步的改进及实验验证,使其更趋完善。结果表明,该法不仅适用于已知混合物,而且适用于未知混合物,是一种比较简捷、快速且行之有效的方法。     

薄层色谱溶剂系统的最优化方法——Ⅵ.均匀设计法的再探讨

就第Ⅱ报及第Ⅴ报提出的用于选取薄层色谱最佳溶剂系统的均匀设计法进行了进一步的改进及实验验证,使其更趋完善。结果表明,该法不仅适用于已知混合物,而且适用于未知混合物,是一种比较简捷、快速且行之有效的方法。     

高效液相色谱与毛细管气相色谱联用技术

本文介绍了一种高效液相色谱与毛细管气相色谱联用的新技术。综述23篇论文的基础上,对联用技术的关键——液相色谱流份向气相色谱转移作了重点介绍。其中柱头进样、恒流溶剂蒸发和共蒸发法是目前常用的流份转移技术。文章指出高效液相色谱与毛细管气相色谱联用技术特别适用于复杂组分和痕量分析,在医药卫生、环保和化工分析中有广阔的前景。     

顶空毛细管气相色谱法测定4-雄烯二酮中的残留溶剂

目的建立顶空毛细管气相色谱法同时测定4-雄烯二酮中甲醇和乙酸乙酯2种残留溶剂的分析方法。方法采用Agilent DB-624毛细管色谱柱(30m×0.32mm×1.8μm),FID检测器,以DMAC为溶剂。结果 2种残留溶剂甲醇和乙酸乙酯在各自的质量浓度范围内呈良好的线性关系(r=0.999 5和0.999 4,n=7),2种残留溶剂甲醇和乙酸乙酯的回收率分别为101.7%和96.9%(RSD为2.04%和4.05%,n=9)。结论该方法操作简单、灵敏度高、适用范围广,适用于4-雄烯二酮中残留溶剂的检测。     

注射用环磷酰胺中残留溶剂的测定

目的建立毛细管柱气相色谱法同时测定注射用环磷酰胺中甲醇、丙酮、二氯甲烷、二氯乙烷和甲苯5种残留溶剂的分析方法。方法采用HP-5毛细管色谱柱(30m×0.53mm,5μm),FID检测器,以DMF为溶剂。结果 5种残留溶剂均能得到很好的分离。峰面积与质量浓度呈良好的线性关系(r>0.999 8),精密度良好。结论该方法简单、准确、灵敏度高,适用于注射用环磷酰胺中残留溶剂的检测。     

毛细管气相色谱法测定氯苄律定中几种有机溶剂残留量

目的建立氯苄律定中几种有机溶剂残留量的测定方法. 方法采用毛细管气相色谱法,色谱柱为PEG-20M石英毛细管柱(0. 25mm×30m),程序升温技术,用内标对比法分离测定氯苄律定中的残留溶剂.结果建立的色谱方法对待测溶剂具有良好的分离度,在所考察的浓度范围内线性关系良好,各溶剂回收率在98.4%～105.1%,检测限1～2ng.结论 本实验建立的色谱方法灵敏、准确,适用于氯苄律定中残留有机溶剂的检测.     

气相色谱法测定盐酸头孢卡品酯中二甲基甲酰胺和苯甲醚残留量方法研究

目的：建立盐酸头孢卡品酯二甲基甲酰胺和苯甲醚溶剂残留量的测定方法.方法：采用HP-INNOWAX毛细管色谱柱,程序升温,FID检测器,载气为氮气,测定盐酸头孢卡品酯中二甲基甲酰胺和苯甲醚的残留量.结果：2种溶剂在所考查的浓度范围内均具有良好的线性关系,相关系数均为0.99以上,2种溶剂的回收率均在90.0％～ 110.0％.结论：本方法专属强,操作简便,结果可靠,适用于残留溶剂的测定.     

气相色谱法测定非诺贝特原料药中残留溶剂苯甲醚的方法

目的：建立以气相色谱法测定非诺贝特原料药中残留溶剂苯甲醚的方法。方法：采用安捷伦6890气相色谱仪、DB-624气相色谱柱进行分析检测,检测器为FID,载气为氮气。结果：采用该方法检测非诺贝特原料药中的苯甲醚精密度好、在一定浓度范围内呈良好的线性方法、回收率为100.49%。结论：该方法简单、准确、灵敏度高,适用于非诺贝特原料药中残留溶剂苯甲醚的含量测定。     

奥拉西坦残留溶剂的测定

目的：建立奥拉西坦原料药中甲醇、乙醇、二氯甲烷、正己烷、环己烷、甲苯、二甲苯和苯八类残留溶剂的测定方法。方法：采用毛细管柱色谱直接进样法,色谱柱DB-624型毛细管柱,柱温采用程序升温,检测器为氢火焰离子化检测器,载气为氮气,柱流量为1.0mL/min-1。结果：8种溶剂均获得基线分离,浓度范围内与峰面积线性关系良好,每个残留溶剂组分平均回收率均符合要求。测定样品3批,甲醇含量均为0.01%,其他七种残留溶剂均未检出。结论：本法专属性强、重复性好、结果可靠、适用于奥拉西坦原料药中残留溶剂的测定。     

六氟异丙醇在难溶性多肽圆二色谱检测中的应用

二级结构是多肽药物发挥药理活性的重要基础,圆二色谱法是测定多肽二级结构最常用的方法,但一些难溶性多肽在检测中往往会遇到溶解度低和溶剂吸收干扰等困难。为了解决难溶性多肽在圆二色谱测定中溶剂选择的困难,文章从溶剂特性及原理出发,提出使用六氟异丙醇作为难溶性多肽的圆二色谱溶剂,并通过对多肽在纯六氟异丙醇及其与PBS混合溶剂的溶解实验和圆二色谱检测,验证了难溶性多肽在上述溶剂中溶解度较高,溶液均一且透明。CD图谱中多肽二级结构特征峰显著、稳定、结构信息充足,且未产生明显的溶剂吸收干扰。这些结果证明了六氟异丙醇可以作为难溶性多肽的良好溶剂,为其圆二色谱检测提供一种新的溶剂选择。     

Über die Verwendung von homogenen azeotropen Gemischen in der Dünnschichtchromatographie 8. Mitt.: Gaschromatographische Untersuchung einiger Fließmittel vor und nach ihrer Verwendung

Homogeneous Azeotropic Mixtures in Thin-layer Chromatography Homogeneous azeotropic mixtures have been analyzed by gas chromatography before and after they were used as solvents in TLC. If polar components were used in a high percentage (> 15%), the composition of solvents was not changed. A certain diminution of polar components has been observed, if their share was low and if there were considerable differences between the components concerning their polarity. The same effect occured, if TLC plates were used which had a layer thickness larger than 0.1 mm.     

Über die Verwendung von homogenen azeotropen Gemischen in der Dünschichtchromatographie, 1. Mitt.

The usefulness of homogeneous azeotropic mixtures in thin layer chromatography has been studied. Several mixtures are qualified for the separation of different classes of substances, for example alkaloids and sulfonamides. TLC with azeotropic solvents leads to especially constant Rf-values and is remarkably economical.     

胶束薄层色谱分离甘草活性成分的影响因素及优化方法

目的:为甘草的胶束薄层色谱指纹图谱寻找最优胶束流动相。方法:首先采用单因子法,寻找影响甘草胶束薄层色谱的影响因素,在此基础上,采用控制加权可变步长单纯形优化法进行甘草胶束薄层色谱指纹图谱的流动相优化。结果:对甘草的胶束薄层色谱分离条件(表面活性剂的种类和含量、醇和酸改性剂的影响等)进行了实验,表明纯胶束薄层色谱的柱效较低,加入醇和酸类改性剂后柱效有明显提高。通过对改性胶束的进一步优化(控制加权可变步长单纯形优化法),得到优化的甘草改性胶束展开剂组成为:0.23 mol.L-1的SDS+16%(v/v)正丁醇+11%(v/v)甲酸。本研究对胶束薄层色谱的一些分离机理亦进行了探讨。结论:胶束薄层色谱的表面活性剂和各添加剂间存在交互作用,需采用合适的优化方法,才能达到分离中药材复杂活性成分群的目的。     

同时检测降脂红曲中酸式和内酯式洛伐他汀的TLC方法的建立

目的 建立同时检测降脂红曲中酸式和内酯式洛伐他汀成分的薄层色谱(TLC)方法。方法 以75%乙醇为提取剂,考察不同上样量、展开剂、显色剂对降脂红曲薄层色谱的影响,从而确认最佳色谱条件,再以HPLC方法进行检测验证。结果 以8μL为上样量,二氯甲烷-丙酮-乙酸(75:25:1)为展开剂,碘蒸气为显色剂,6批降脂红曲在与酸式、内酯式洛伐他汀对照品相同的位置上均呈现相同颜色斑点,且斑点清晰、分离度好。HPLC检测结果与TLC检测结果相符。结论 所建立的TLC方法具有简单、快速、低成本、重复性高的特点,可用于降脂红曲的质量控制。     

吗啡类药物成瘾者尿液的薄层层析检测

本文报告１５７例吗啡类药物成瘾者采取不同方法戒断或瘾的尿样，经酸性水解后有机溶剂提取，薄层层析定性检查，结果表明本法准确可靠，简便快速。不需特殊设备，适用于基层单位。     

清火片薄层色谱鉴别提高

目的建立清火片薄层色谱鉴别。方法采用薄层色谱法（TLC）对处方中的主要成分大青叶进行鉴别。结果在TLC图谱中可检出大青叶的特征斑点。结论该方法优于现存的药品标准鉴别方法,简便易行,重现性好,为清火片提供了一种质量控制方法。     

Marquris法和薄层色谱法用于海洛因滥用者尿液中吗啡检测的对比研究

本文应用Marquris法和薄层色谱法,对110例海洛因滥用者戒毒期间尿液中吗啡进行对比检测。结果:Marquris法测出阳性35例,符合率为47.6％,薄层色谱法测出阳性63例符合率100％,差异有高度显著性(P<0.01)。说明薄层色谱法的敏感性、可靠性明显优于Marquris法。     

System evaluation and substance identification in systematic toxicological analysis by the mean list length approach

In systematic toxicological analyses (STA), analytical methods are needed with a high Identification Power. The mean list length (MLL) approach, which is an improved and extended version of the Identification Power concept, provides an objective tool for the evaluation and optimum choice of analytical methods for STA. The MLL approach is elucidated and applied to the screening for basic drugs by thin layer chromatography (TLC) and gas-liquid chromatography (GLC). Its usefulness for TLC and GLC systems for the identification of these basic drugs has been evaluated for both single systems and combinations of systems. The MLL approach is also substance directed and can be applied to computerized data searches and substance identification. The method is applicable for single analytical systems and combinations of systems. Mixtures of substances can also be handled.     

止痛顺气胶囊的薄层色谱鉴别简

目的建立止痛顺气胶囊的薄层色谱鉴别方法。方法采用薄层色谱法对处方中的黄柏、陈皮、肉桂进行定性鉴别。结果薄层色谱法可鉴别出处方中的黄柏、陈皮、肉桂。结论该方法专属性强、重现性好,可用于止痛顺气胶囊的质量控制。     

Historical study of separation technology innovation in the field of pharmaceutical science

The separation of organic compounds has been carried out using the method of distillation and recrystallization since the 17th century.1st separation technology innovation (1950s to 1960s). After World War II, the science of separating organic compounds evolved to the use of paper or column chromatography. 2nd separation technology innovation (1960s to 1980s). In the 1960s, thin-layer chromatograpy (TLC) was developed. TLC is a convenient analytical technique for organic compounds. Separation methods for organic compounds using column chromatography and preparative TLC were carried out as practical applications. Gas chromatography (GC) was also introduced in the 1960s. GC is a useful analytical method for a mixture of various volatile organic compounds. Many GC instruments with new kinds of sensors were developed. Gas chromatography of nonbenzenoid organometallic compounds and metal complexes was successfully conducted by the author. 3rd separation technology innovation (1980s to 1990s). In the 1980s, high-performance liquid-chromatography (HPLC) was developed. HPLC analytical methods were useful for various kinds of organic compounds. In the 1990s, LC-MS and LC-NMR instruments were introduced for biomedical products. 4th separation technology innovation (1990s to present). Several new ionization methods for mass-spectrometry (electrospray, matrix-aided lazer desorption ionization, etc) are applied for proteins and biomedical products. Several new separation technologies (supercritical field chromatography, capillary electrophoresis, field-flow fractionization, etc.) are now being developed.