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

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.