小花棘豆生物碱薄层色谱分析及GC-MS检测

Determination of Alkaloids of Oxytropis glabra DC by TLC and GC-MS

为确定小花棘豆生物碱的种类,建立小花棘豆生物碱指纹图谱,为其毒性作用机理及药理作用研究提供理论依据。用溶剂萃取法提取小花棘豆各极性段生物碱,并通过薄层层析进行初步分析;将萃取量少、小极性的氯仿、乙酸乙酯部分生物碱合并进行硅胶正相柱层析分离,薄层色谱跟踪检测;将洗脱量少、改良碘化铋钾显色明显的洗脱部分合并,应用微量GC-MS进行分析鉴定。结果表明,各萃取段粗碱经不同展开体系薄层展开H2O2/10%醋酐无水乙醇/Ehrlich’s试剂显色较佳,且各显色点呈斑点性强;将氯仿、乙酸乙酯部分生物碱经柱层析分离得到的改良碘化铋钾显色明显的组分合并,经GC-MS分析鉴定出16种生物碱,相对含量大于3%以上的有3种,占总提取物的26.72%,相对含量大于2%的有1种,相对含量大于1%的有5种,皆属首次从此植物中发现。

In order to determine the species of alkaloids,to develop the fingerprints and to provide theoretical basis for the toxic mechanism and pharmacological action of Oxytropis glabra DC,the alkaloids of different polarity sections were extracted by solvent extraction and analyzed by TLC（thin layer chromatography）;The chloroform and ethyl acetate extractions were little and combined and separated by silica gel positive column chromatography.The elution was monitored by TLC and the section well colored by modified Dragendorff reagent was identified by GC-MS（gas chromatography-mass spectrometry）.The results showed that the alkaloids of different extraction had an excellent color by H2O2/10% Acetic anhydride absolute alcohol/Ehrlich＇s reagent on plate developed by different developing systems.The sections separated by column chromatography and well colored by modified Dragendorff reagent were combined and 16 species of alkaloids were identified by GC-MS.The relative percentage content of three compounds occupied 26.72% of all extractions were above 3%,one compound was above 2%,five compounds were higher than 1%,all of which were first detected.