基于核壳色谱技术快速测定厚朴药典指标成分和厚朴酚及厚朴酚的含量

Rapid Determination of the Contents of Honokiol and Magnolol in Magnolia officinalis Based on Core-shell Chromatography

目的建立中药厚朴药典指标成分和厚朴酚及厚朴酚的快速含量测定方法。方法样品经甲醇超声提取后,基于核壳色谱技术采用高效液相色谱法测定。色谱柱为Agilent Poroshell EC-C_(18)(50 mm×4.6 mm,2.7μm),流动相为甲醇-0.1%甲酸水(78∶22),流速为1 mL·min^(-1),柱温为35℃,检测波长为294 nm。结果本方法可在8 min内完成厚朴中和厚朴酚及厚朴酚的测定(5 min样品提取和3 min色谱分析)。和厚朴酚、厚朴酚分别在0.0427~4.4492 mg·mL^(-1)、0.0428~4.4531 mg·mL^(-1)范围内线性关系良好,相关系数均为0.9999;精密度、重复性良好,RSD均小于2.0%;加样回收率为94.89%~104.89%(和厚朴酚RSD=2.12%,厚朴酚RSD=1.94%,n=6);对照品和供试品溶液在室温下放置24 h内稳定。10批不同来源的厚朴中和厚朴酚、厚朴酚含量分别为0.64%~3.93%、1.22%~4.71%。结论建立的色谱分析方法简便、快速、准确,有助于提升厚朴样品的检测效率。

OBJECTIVE To develop a HPLC method for rapid determination of honokiol and magnolol in Magnolia officinalis based on core-shell chromatography.METHODS The samples were prepared by ultrasonic extraction with methanol.The HPLC method was carried out on Agilent Poroshell EC-C_(18) column(50 mm×4.6 mm,2.7μm)with elution of methanol-0.1% formic acid(78∶22)ata flow rate of 1 mL·min^(-1).The column temperature was 35℃and the detection wavelength was 294 nm.RESULTS The method wasfinished within 8 min(5 min for sample preparation and 3 min for HPLC).Honokiol and magnolol had good linear relationships in therange of 0.0427-4.4492 mg·mL^(-1) and 0.0428-4.4531 mg·mL^(-1),and the correlation coefficients were both 0.9999.The precision and repeatability were good(RSD<2.0%).The sample recovery was 94.89%-104.89%(honokiol RSD=2.12%,magnolol RSD=1.94%,n=6).The reference and sample solution were stable within 24 hours at room temperature.The contents of honokiol and magnolol in ten batches of Magnolia officinalis were 0.64%-3.93% and 1.22%-4.71%,respectively.CONCLUSION The established method is simple,rapid,and accurate,which is helpful to improve the detection efficiency of Magnolia officinalis samples.