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[龙胆中龙胆苦苷和马钱子酸的含量及其指纹图谱]

[Content of gentiopicroside and loganic acid in Radix gentianae and their fingerprints].

作者信息

Li Wen-Long, Chen Jun-Hui, Yin Yue-Fen, Wu Feng-Qi, Yang Bai-Juan, Yang Huang-Hao, Wang Xiao-Ru

机构信息

Qingdao Key Lab of Analytical Technology Development and Standardization of Chinese Medicines, First Institute Oceanography of State Oceanic Administration People's Republic of China, Qingdao 266061, China.

出版信息

Yao Xue Xue Bao. 2007 May;42(5):566-70.

Abstract

To develop a HPLC-DAD-ESI-TOF/MS analysis method for the determination of gentiopicroside and loganic acid in Radix gentianae samples and for the research of their fingerprints. The samples were extracted using ASE for 10 min under 100 degrees C and 9.65 MPa, and divided into water phase and chloroform phase and analyzed them with HPLC-DAD-ESI-TOF/MS method respectively. Based on this method, the HPLC fingerprints of Radix gentianae were established. Comparing the spectrogram and mass spectrum of the chromatogram peak with the reference value, three compounds in water phase were identified as gentiopicroside, asafetida acid and loganic acid. There is no report of the compounds in chloroform phase. The content of gentiopicroside and loganic acid in samples of different groups were determined, separately. The fingerprints were compared by the software of the similarity evaluation system for chromatographic fingerprint. The water phase fingerprint congruence coefficients of samples from six different areas were above 0.90, however, the chloroform phase fingerprint congruence coefficients were within 0.62 -0.99. This method can be used for determination of potent component in Radix gentianae and its quality control. Radix gentianae from different producing areas have the largest diversities, and the diversities embodied in the content of chloroform phase compounds.

摘要

建立一种高效液相色谱-二极管阵列检测器-电喷雾电离-飞行时间质谱(HPLC-DAD-ESI-TOF/MS)分析方法,用于测定龙胆样品中龙胆苦苷和马钱子酸的含量,并研究其指纹图谱。样品采用加速溶剂萃取(ASE)在100℃、9.65MPa条件下萃取10min,分为水相和氯仿相,分别用HPLC-DAD-ESI-TOF/MS方法进行分析。基于该方法,建立了龙胆的HPLC指纹图谱。将色谱峰的光谱图和质谱图与参考值进行比较,确定水相中三种化合物为龙胆苦苷、阿魏酸和马钱子酸。氯仿相中化合物未见报道。分别测定不同组样品中龙胆苦苷和马钱子酸的含量。采用色谱指纹图谱相似度评价系统软件对指纹图谱进行比较。六个不同产地样品的水相指纹图谱相似度系数均在0.90以上,而氯仿相指纹图谱相似度系数在0.62 - 0.99之间。该方法可用于龙胆有效成分的测定及其质量控制。不同产地的龙胆差异最大,差异体现在氯仿相化合物的含量上。

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