小茴香中反式茴香脑的含量测定及其变化规律研究

Determination of the trans-anethole content in fructus foeniculi and its variation rule

关键词:  小茴香  超高效液相色谱法  反式茴香脑

Key words:  Fructus Foeniculi  ultra performance liquid chromatography  trans-anethole

摘要:

[目的]构建基于超高效液相色谱法（UPLC）的小茴香中反式茴香脑的含量测定方法，系统研究了小茴香药材（生品）及其粉末中反式茴香脑随放置不同时间的含量变化规律。[方法]色谱柱ACQUITY UPLC^®BEH C18（2.1 mm×50 mm，1.7 μm），以甲醇0.1%-甲酸水（55：45）为流动相，检测波长为254 nm，流速为0.3 mL/min，柱温为40℃，样品箱温度5℃，进样量为2 μL。按规定时间采集小茴香药材（生品）及其粉末在室温条件下放置不同时间的样本，分析系列样品中反式茴香脑的含量。[结果]小茴香中反式茴香脑含量测定方法学研究符合2015年版《中华人民共和国药典》中《药品质量标准分析方法验证指导原则》的相关要求；小茴香药材（生品）与盐制品中反式茴香脑含量差异较大，合格率较低；盐制品在炮制过程中反式茴香脑含量略有变化。在室温条件下小茴香药材（生品）中反式茴香脑的含量在规定放置时间内基本稳定；药材粉碎后反式茴香脑含量随放置时间延长不断下降。[结论]本方法样品前处理简便，重现性良好，分析速度快，结果准确可靠，可用于小茴香中反式茴香脑的含量测定及其变化规律研究。

Abstract:

[Objective] To establish a method for determining the trans-anethole content in Fructus Foeniculi by ultra-performance liquid chromatography (UPLC). The variation rule of trans-anethole content in Fructus Foeniculi (raw) and its powder over time was systematically studied.[Methods] The analysis was performed on ACQUITY UPLC^®BEH C18 Column (2.1 mm×50 mm,1.7 μm) with the mobile phase of methanol-0.1% formic acid (55:45) at 0.3 mL/min. The detection wavelength was 254 nm. The column temperature was fixed at 40℃,the temperature of sample injector was 5℃ and the injection volume was 2 μL. Samples of Fructus Foeniculi (raw) and its powder placed at room temperature were collected at the specified times,and the trans-anethole content of which was analyzed.[Results] The methodological study for determination of trans-anethole in Fructus Foeniculi satisfied the requirements of Validation Guidelines for Analytical Method of Pharmaceutical Quality Standard from ChP. The trans-anethole content in Fructus Foeniculi (raw) and its salt product was quite different,almost half of which cannot meet the standard released by ChP. The trans-anethole content in the salt product was slightly changed during the processing. Under the condition of room temperature,the trans-anethole content in Fructus Foeniculi (raw) was basically stable within the specified storage time. However,the trans-anethole content decreased rapidly within the specified storage time after the Medicinal herbs were pulverized.[Conclusion] The method has the advantages of simple pretreatment,good reproducibility,fast analysis,accurate and reliable result,which can be used for studying the trans-anethole content in Fructus Foeniculi and its variation rule.