龙涎香中龙涎香醇的制备及其含量测定研究  

Study on the Preparation and Content Determination of Ambrein in Ambergris

作　　者：杜佳丽[1] 宋卓悦 张丹雁[1] 杨丽 DU Jiali;SONG Zhuoyue;ZHANG Danyan;YANG Li(School of Pharmaceutical Sciences,Guangzhou University of Chinese Medicine,Guangzhou 510006 Guangdong,China;Clinical Medical College of Acupuncture Moxibustion and Rehabilitation,Guangzhou University of Chinese Medicine,Guangzhou 510006 Guangdong,China)

机构地区：[1]广州中医药大学中药学院,广东广州510006 [2]广州中医药大学针灸康复临床医学院,广东广州510006

出　　处：《中药新药与临床药理》2021年第9期1353-1358,共6页Traditional Chinese Drug Research and Clinical Pharmacology

摘　　要：目的制备龙涎香醇对照品,建立龙涎香醇含量测定方法。方法龙涎香醇通过石油醚超声提取、硅胶柱层析、丙酮洗涤、半制备液相色谱的方法制备。采用气相-质谱联用(GC-MS)法测定龙涎香醇的纯度,采用核磁共振(NMR)及超高液相-质谱联用(UPLC-MS)法,对龙涎香醇的结构进行确证。采用高效液相-蒸发光散射(HPLC-ELSD)法,建立龙涎香醇的检测方法并评价龙涎香的质量。结果所制备的龙涎香醇纯度为95.12%,符合国家对照品标准要求。13批龙涎香样品中龙涎香醇的含量介于29.2%~63.6%之间。结论建立了龙涎香醇对照品制备方法及龙涎香醇含量测定方法,可为龙涎香的真伪鉴别提供准确、可量化的方法。Objective The purpose was to prepare ambrein standard substance and establish detection method for ambrein.Methods Ambrein was prepared by ultrasonic extraction using petroleum ether,silica gel column chromatography,acetone washing,and semi-preparative high performance liquid chromatography.Gas chromatography-mass spectrometry(GC-MS)method was used to determine the purity of amberin.Nuclear magnetic resonance(NMR)and ultra-high liquid chromatography-mass spectrometry(UPLC-MS)methods were used to confirm the chemical structure of amberin.The high performance liquid phase-evaporative light scattering detection(HPLC-ELSD)method was used to establish detection method for amberin and evaluate the quality of ambergris.Results The purity of the obtained amberin was 95.12%,which met the requirements of the national reference standard.The amberin contents in 13 batches of ambergris were between 29.2%and 63.6%.Conclusion The amberin standard preparation method and amberin content determination method were established,which provided accurate and quantifiable method for the authenticity of ambergris.

关 键 词：龙涎香 龙涎香醇 高效液相-蒸发光散射法 含量测定 

分 类 号：R284.1[医药卫生—中药学] R284.2[医药卫生—中医学]