HPLC-DAD-MS检测川芎和日本川芎中的川芎嗪  

Assay of Tetramethylpyrazine in Szechwan Lovage Rhizome and Cnidium Rhizome by HPLC-DAD-MS

作　　者：洪远林[1] 金玉青 姚艺新 林懋怡 魏伯平 姜卫东 吕光华[1] 

机构地区：[1]中药资源系统研究与开发利用国家重点实验室培育基地/中药材标准化教育部重点实验室/成都中医药大学药学院,四川成都611137 [2]成都市海通药业有限公司,四川成都611137 [3]四川省食品药品检验检测院,四川成都610097

出　　处：《中药材》2015年第1期36-40,共5页Journal of Chinese Medicinal Materials

基　　金：四川省中医药管理局科技专项(2010-08);成都中医药大学药学院本科学生科技发展基金项目

摘　　要：目的：建立川芎药材中川芎嗪的检测方法,测定川芎和日本川芎中的川芎嗪,阐明川芎嗪是否存在及其含量高低。方法：HPLC-DAD-MS法,色谱柱为Waters Symmetry C18（250 mm×4.6 mm,5μm）,流动相为甲醇-乙腈-水（27∶1∶72）,流速1.0 m L/min,柱温35℃,检测波长280 nm;MS采用电喷雾正离子化模式检测。结果：在37份川芎和日本川芎样品中,有11份发现川芎嗪,占29.7%,平均含量为2.19μg/g（n=11）。其中,在27份川芎样品中,有6份检测出川芎嗪（0.60~11.75μg/g）;在10份日本川芎样品中,有5份检测出川芎嗪（0.61~3.05μg/g）。川芎嗪的存在与药材产地、性状特征、加工及贮藏方法之间无相关性,可能与土壤中微生物有关。结论：建立的方法可准确测定川芎和日本川芎中的川芎嗪;这两种药材中川芎嗪的含量很低,不是二者的主要功效成分,也不宜作为其质量评价的指标成分。Objective： To quantify the amount of tetramethylpyrazine in Szechwan Lovage Rhizome（Chuanxiong,the rhizome of Ligusticum chuanxiong Hort.,CX） and Cnidium Rhizome（Japanese Chuanxiong,the rhizome of Cnidium officinale Makino,JCX） for quality assessment. Methods： An HPLC-DAD-MS technique was employed to detect tetramethylpyrazine in 27 CX and 10 JCX samples. Tetramethylpyrazine was separated on a Waters Symmetry C18column（250 mm × 4. 6 mm,5 μm）. The mobile phase was methanolacetonitrile-water（27∶ 1∶ 72） at a flow rate of 1. 0 m L/min. The column temperature was 35 ℃. DAD detection wavelength was 280 nm,while electrospray ionization detector was set at positive mode to collect MS spectrum. Results： In the total of 37 herb samples,11 samples were found to contain tetramethylpyrazine with the mean amount of 2. 19 μg/g（n = 11）. 6 of 27 CX samples and 5 of 10 JCX sample were found the existence of tetramethylpyrazine with the amount of 0. 60 ~ 11. 75 μg/g and 0. 61 ~ 3. 05 μg/g,respectively. The correlation was not found between tetramethylpyrazine and the cultivation area,morphological character,processing or storage method for CX and JCX samples. It was possible that tetramethylpyrazine resulted from the microbes in soil. Conclusion： The developed method is accurate to quantify tetramethylpyrazine in CX and JCX herbs. Both the two herbs indeed contain tetramethylpyrazine,but it is not suitable to be a chemical marker to assess the quality of CX and JCX owing to low content.

关 键 词：川芎 日本川芎 川芎嗪 含量测定 高效液相色谱 

分 类 号：R284.1[医药卫生—中药学]