气相色谱-质谱法测定当归片和当归超微片中藁本内酯的含量比较研究  

Comparative study on determining the content of Angelica tablets and ultra tablets of ligustilide by gas chromatography-mass spectrometer

作　　者：李越峰[1,2] 司昕蕾 牛江涛 曹瑞[1,2] 边甜甜 刘岩峥[3] LI Yue-feng;SI Xin-lei;NIU Jiang-tao;CAO Rui;BIAN Tian-tian;LIU Yan-zheng(University of Traditional Chinese Medicine of Gansu,Lanzhou 730000,China;Key Laboratory of Standard and Quality of Chinese Medicine Research of Gansu,Lanzhou 730000,China;Gansu Provincial Cancer Hospital,Lanzhou 730050,China)

机构地区：[1]甘肃中医药大学,兰州730000 [2]甘肃省中药质量与标准研究重点实验室,兰州730000 [3]甘肃省肿瘤医院,兰州730050

出　　处：《中国临床药理学杂志》2018年第22期2643-2645,共3页The Chinese Journal of Clinical Pharmacology

基　　金：国家自然科学基金资助项目(81460611);国家教育部科学技术研究重点基金资助项目(212186);甘肃省自然科学基金资助项目(2010:1010RJZA212; 2014:145RJZA076);甘肃省财政厅高校基本科研业务费专项基金资金项目(2013-2);兰州市科技局基金资助项目(2014-1-188);甘肃省中医药管理局科研课题基金资金项目(GZK-2015-57)

摘　　要：目的建立当归片与当归超微片中藁本内酯含量测定快速灵敏的检测方法。方法用超声提取法进行当归片剂中藁本内酯的提取,以石油醚和正己烷为提取溶剂,用气相色谱-质谱法(GC-MS)测定当归片剂中藁本内酯的含量并分析藁本内酯的稳定性。结果藁本内酯进样量在0. 30～10. 00 mg·m L^(-1)内呈良好的线性关系,响应值与浓度的回归方程为:Y=3. 94×10~7X-1. 63×10~7(R^2=0. 9987)。在其他条件相同时,石油醚提取当归超微片中藁本内酯较提取当归片的含量高,正己烷提取当归超微片中藁本内酯的含量高于其他溶剂,当归片正己烷提取液的藁本内酯含量最低。结论不同提取溶剂会影响当归片剂中藁本内酯的含量。本文建立的GC-MS选择离子监测外标定量方法,具有灵敏、快速、准确的特点,可供当归片与当归超微片的质量控制及藁本内酯的含量测定。Objective To establish a rapid and sensitive method for the determination of ligustilide in Angelica sinensis and Angelica ultramicron tablets. Methods The extraction of ligustilide in Angelica sinensis tab- lets was carried out by ultrasonic extraction. The content of ligustiiide in Angelica sinensis tablets was determined by gas chromatography -mass spectrometer（ GC -MS）with petroleum ether and n -hexane as extraction solvent. The stability of ligustilide in Angelica sinensis was analyzed. Results The injection amount of ligustilide showed a good linear rela- tionship in the range of 0. 30 - 10. 00 mg·mL^-1. The regression equa- tion of response value and concentration was： Y=3.94 × 10^7X - 1.63×10^7（R^2 =0. 9987）. When the other conditions were the same, the con- tent of ligustilide in the extract of Angelica sinensis was slightly higher than that of the angelica tablets. The content of ligustilide in the hexane extraction of Angelica ultrafine tablets was higher than that of other sam- pies. The content of ligusticide in the hexane extract of Angelica sinensis is the lowest. Conclusion Different extraction solvents will affect the content of ligustilide in Angelica tablets. The GC -MS selective ion mo- nitoring external standard quantitative method established in this paper is sensitive, rapid and accurate, and can be used for the quality control of Angelica sinensis and Angelica ultramicrochips and the determination of ligustilide content.

关 键 词：当归片 当归超微片 藁本内酯 气相色谱-质谱法 面积外标法 

分 类 号：R28[医药卫生—中药学]