HPLC-DAD法同时测定五味子中10种木脂素成分的含量

Quantitative Determination of Ten Lignans Constituents from Schisandra chinensis Baill.by HPLC-DAD

目的:建立同时测定五味子中10种特定木脂素类成分含量的方法。方法:采用高效液相色谱法分离10种特定木脂素成分,以菲罗门公司Luna C18(250 mm×4.6 mm,5μm)为色谱柱,采用乙腈-水为流动相系统,使用梯度洗脱模式(0~20 min,45%B→65%B;20~26 min,65%B;26~50 min,65%B→75%B),检测波长为220 nm,流速为0.8 mL/min,进样量为5μL。结果:五味子中10种特定木脂素成分的线性范围分别为20.0~200.0μg/mL(r=0.9999),2.0~20.0μg/mL(r=0.9998),4.0~40.0μg/mL(r=0.9999),13.3~133.3μg/mL(r=0.9999),4.0~40.0μg/mL(r=0.9995),6.3~62.5μg/mL(r=0.9999),6.7~66.7μg/mL(r=1.0000),4.0~40.0μg/mL(r=0.9999),4.0~40.0μg/mL(r=0.9997)和10.0~100.0μg/mL(r=1.0000);平均回收率分别为99.3%(RSD=2.5%),100.2%(RSD=2.5%),102.1%(RSD=1.6%),98.5%(RSD=2.4%),96.5%(RSD=3.2%),99.4%(RSD=2.8%),99.1%(RSD=2.7%),97.5%(RSD=2.5%),101.9%(RSD=3.1%)和100.6%(RSD=3.5%)。结论:采用该方法测定了12批五味子中10种木脂素成分的含量,该方法简便、快速、准确,可用于五味子中药材及中药制剂中木脂素类成分的质量控制。

Objective:To establish a method of simultaneous determination of ten lignans in Schisandra chinensis by high-performance liquid chromatography.Methods:5μL of the sample was injected into LC system and separated on a Luna C18 column(250 mm×4.6 mm,5μm)at 30°C using a gradient elution(the gradient started from 45%acetonitrile to 65%within 20 min,kept 65%acetonitrile for 6 min,then changed from 65%acetonitrile to 75%within 24 min).The flow rate maintained 0.8 mL/min.The UV detector was at 220 nm.Results:The calibration curves of the 10 lignans in Schisandra chinensis were respectively 20.0~200.0μg/mL(r=0.9999),2.0~20.0μg/mL(r=0.9998),4.0~40.0μg/mL(r=0.9999),13.3~133.3μg/mL(r=0.9999),4.0~40.0μg/mL(r=0.9995),6.3~62.5μg/mL(r=0.9999),6.7~66.7μg/mL(r=1.0000),4.0~40.0μg/mL(r=0.9999),4.0~40.0μg/mL(r=0.9997)and 10.0~100.0μg/mL(r=1.0000);The average recoveries were respectively 99.3%(RSD=2.5%),100.2%(RSD=2.5%),102.1%(RSD=1.6%),98.5%(RSD=2.4%),96.5%(RSD=3.2%),99.4%(RSD=2.8%),99.1%(RSD=2.7%),97.5%(RSD=2.5%),101.9%(RSD=3.1%)and 100.6%(RSD=3.5%).Conclusion:The method can be successfully applied to quantify the ten lignans in 12 samples of Schisandra chinensis from different sources.The method is simple,rapid and accurate.It can be used for the quality control of Schisandra chinensis.