摘要
目的:建立重楼中皂苷类成分的薄层色谱-质谱联用分析法。方法:样品经乙醇回流提取,点样于硅胶G预制板上,以三氯甲烷-乙酸乙酯-甲醇-水(17∶40∶21∶10)10℃以下放置的下层溶液为展开剂展开,喷以10%硫酸乙醇溶液,于105℃加热至条斑清晰,置紫外光灯(365 nm)下检视并成像。使用重楼皂苷Ⅰ、重楼皂苷Ⅱ、重楼皂苷Ⅵ和重楼皂苷Ⅶ对照品以及四极杆飞行时间串联质谱(QTof MS)进行成分识别。结果:紫外光灯(365 nm)下,重楼色谱可见23个荧光条斑,其中以薯蓣皂苷元为母核的皂苷显棕色,以偏诺皂苷元为母核的皂苷显淡蓝色,使用对照品和质谱仪共鉴别8个条斑,对应成分为重楼皂苷Ⅰ、重楼皂苷Ⅱ、重楼皂苷Ⅲ、重楼皂苷Ⅴ、重楼皂苷Ⅵ、重楼皂苷Ⅶ、重楼皂苷D和纤细薯蓣皂苷。结论:该法简便、专属,适用于重楼的快速鉴别并可为重楼药材整体质量评价提供参考。
Objective: To establish a method for identification of saponins in Paridis Rhizoma by thin layer chromatography -mass spectrometry. Methods: The samples were extracted by reflux with ethanol, and the chromatography was carried out on silica gel G pre - coated plates, using the lower layer of a mixture of chloroform - ethyl ace- tate -methanol -water( 17:40: 21: 10) as mobile phase; the temperature was controlled below 10 ℃, and the samples were examined in ultraviolet light at 365 nm after derivatization with 10% sulfuric acid alcoholic solution. The bands for compounds were identified by reference substances of Chonglou saponin I , Chonglou saponin Ⅱ , Chonglou saponin VI and Chonglou saponin Ⅷ and quadrupole time of flight mass spectrometry(QTofMS). Results: In the chromatogram of Paridis Rhizoma, twenty three bands were visualized by UV light at 365 nm, eight bands were identified, including Chonglou saponin I , Chonglou saponin Ⅱ , Chonglou saponin m, Chonglou saponin V, saponin Ⅵ, Chonglou saponin Ⅶ, Chonglou saponin D amd gracillin. The bands of diosgenin were brown, and the bands of pennogenin were light blue. Conclusion: The established method is simple and specific, which can be used for rapid detection and quality evaluation of Paridis Rhizoma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第8期1495-1499,共5页
Chinese Journal of Pharmaceutical Analysis
基金
国家食药总局进口药材标准增修订专项(No.JKYC2012-14)