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

[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,1.7μm),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 m L/min,柱温为40℃,样品箱温度5℃,进样量为2μL。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。

[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.