薄层色谱法分离色素是大学有机化学实验中提取、分离与鉴定部分的代表性实验。针对按照教材所述的方法进行实验结果达不到理论效果的问题,我们对菠菜叶中色素的提取和分离的影响因素进行了研究。提取剂种类和配比、提取时间、提取剂用...薄层色谱法分离色素是大学有机化学实验中提取、分离与鉴定部分的代表性实验。针对按照教材所述的方法进行实验结果达不到理论效果的问题,我们对菠菜叶中色素的提取和分离的影响因素进行了研究。提取剂种类和配比、提取时间、提取剂用量等因素对影响色素提取效果的研究结果表明,最佳的提取条件为:提取剂为乙醇-丙酮(2∶1),提取时间10 min,提取剂用量20 m L。展开剂种类和配比对影响色素分离效果的研究表明,最佳的二元展开剂体系是(2∶1)^(1.5∶1)的石油醚-乙酸乙酯和(2.5∶1)^(2∶1)的石油醚-丙酮体系。展开更多
[Objectives] To establish a simple and rapid,specific and reproducible thin layer chromatography( TLC) method,and accordingly establish a thin layer identification method for quality control of Glycyrrhiza uralensis. ...[Objectives] To establish a simple and rapid,specific and reproducible thin layer chromatography( TLC) method,and accordingly establish a thin layer identification method for quality control of Glycyrrhiza uralensis. [Methods] According to the physical and chemical properties,components of Glycyrrhiza uralensis were identified by thin layer chromatography. According to Veterinary Pharmacopoeia of the People's Republic of China 2010( Volume Ⅱ) and related literature report,the thin layer chromatography identification method was studied and improved for Glycyrrhiza uralensis.[Results] When the preparation method for test sample solution was 6g Glycyrrhiza uralensis added with 30 mL saturated n-butanol,ultrasonic processing 20 min,filtered,filtrate dried,added 3 mL methanol and obtained Glycyrrhiza uralensis test sample solution. Then,chloroform-methanol-formic acid-ethyl acetate( 10∶ 3∶ 2∶ 3) as developing solvent,clear spot with high degree of separation and reproducibility could be obtained,and can be used for thin layer chromatography identification of ammonium glycyrrhetate in Glycyrrhiza uralensis.[Conclusions] The modified method omitted the step of ether treatment of samples,and directly adopted saturated n-butanol to extract components. It does not influence the detection of chromatographic spots,and solves the issue of sample gelatinizing sticking and filtration,simplifies the test process,and reduces the harm to human body.展开更多
针对油酸提纯,设计薄层色谱展开剂比例的正交试验,优化了正己烷-乙酸乙酯-乙酸的体积比,采用相对标准偏差检验了薄层色谱法分离工业油酸的精密度。将展开剂的比例用作柱层析洗脱液,考察了硅胶装填高度、上样量对柱层析法分离油酸质量分...针对油酸提纯,设计薄层色谱展开剂比例的正交试验,优化了正己烷-乙酸乙酯-乙酸的体积比,采用相对标准偏差检验了薄层色谱法分离工业油酸的精密度。将展开剂的比例用作柱层析洗脱液,考察了硅胶装填高度、上样量对柱层析法分离油酸质量分数和收率的影响,确定柱层析分离过程条件。测试了层析柱循环使用的效果,为油酸提纯的工业化研究提供依据。结果表明:洗脱液正己烷-乙酸乙酯-乙酸的最佳体积比为85∶15∶8,方法稳定可靠;在硅胶的装填高度为40 cm,工业油酸的上样量为1.1 m L时,油酸的分离效果最好。在此条件下,油酸的质量分数达到88.74%,收率达到82.53%。展开更多
文摘薄层色谱法分离色素是大学有机化学实验中提取、分离与鉴定部分的代表性实验。针对按照教材所述的方法进行实验结果达不到理论效果的问题,我们对菠菜叶中色素的提取和分离的影响因素进行了研究。提取剂种类和配比、提取时间、提取剂用量等因素对影响色素提取效果的研究结果表明,最佳的提取条件为:提取剂为乙醇-丙酮(2∶1),提取时间10 min,提取剂用量20 m L。展开剂种类和配比对影响色素分离效果的研究表明,最佳的二元展开剂体系是(2∶1)^(1.5∶1)的石油醚-乙酸乙酯和(2.5∶1)^(2∶1)的石油醚-丙酮体系。
基金Supported by the Famous Teacher Program for High-level Talent Special Support Project of Chongqing City[Yu Wei Zu(2015)No.120]
文摘[Objectives] To establish a simple and rapid,specific and reproducible thin layer chromatography( TLC) method,and accordingly establish a thin layer identification method for quality control of Glycyrrhiza uralensis. [Methods] According to the physical and chemical properties,components of Glycyrrhiza uralensis were identified by thin layer chromatography. According to Veterinary Pharmacopoeia of the People's Republic of China 2010( Volume Ⅱ) and related literature report,the thin layer chromatography identification method was studied and improved for Glycyrrhiza uralensis.[Results] When the preparation method for test sample solution was 6g Glycyrrhiza uralensis added with 30 mL saturated n-butanol,ultrasonic processing 20 min,filtered,filtrate dried,added 3 mL methanol and obtained Glycyrrhiza uralensis test sample solution. Then,chloroform-methanol-formic acid-ethyl acetate( 10∶ 3∶ 2∶ 3) as developing solvent,clear spot with high degree of separation and reproducibility could be obtained,and can be used for thin layer chromatography identification of ammonium glycyrrhetate in Glycyrrhiza uralensis.[Conclusions] The modified method omitted the step of ether treatment of samples,and directly adopted saturated n-butanol to extract components. It does not influence the detection of chromatographic spots,and solves the issue of sample gelatinizing sticking and filtration,simplifies the test process,and reduces the harm to human body.
文摘针对油酸提纯,设计薄层色谱展开剂比例的正交试验,优化了正己烷-乙酸乙酯-乙酸的体积比,采用相对标准偏差检验了薄层色谱法分离工业油酸的精密度。将展开剂的比例用作柱层析洗脱液,考察了硅胶装填高度、上样量对柱层析法分离油酸质量分数和收率的影响,确定柱层析分离过程条件。测试了层析柱循环使用的效果,为油酸提纯的工业化研究提供依据。结果表明:洗脱液正己烷-乙酸乙酯-乙酸的最佳体积比为85∶15∶8,方法稳定可靠;在硅胶的装填高度为40 cm,工业油酸的上样量为1.1 m L时,油酸的分离效果最好。在此条件下,油酸的质量分数达到88.74%,收率达到82.53%。
