五味子药材中醇甲和酯甲的测定

Determination of schisandrin and schisantherin A in fructus schisandra chinensis

五味子以100%甲醇溶解,用超声波清洗器提取20 min,建立一种同时对五味子药材中五味子醇甲和酯甲定性和含量测定的HPLC-MS方法。色谱条件：色谱柱ZORBAXEclipse XDB-C18（150 mm×4.6 mm i.d.,5μm）,流动相甲醇-水（体积比65∶35）,流速0.8 mL/min,检测波长220 nm,柱温20℃,进样量20μL。质谱条件：电喷雾离子源（ESI＋源）,扫描范围（m/z）：300-600,干燥气温度350℃,干燥气流速8.0 mL/min,雾化气压力275.8 kPa。结果表明,五味子醇甲和酯甲分别在1.3~83.2μg和1.04~66.56μg浓度范围内具有良好的线性关系,相关系数r分别为0.998和0.997,平均加标回收率分别为100.7%和99.7%,RSD均小于2%。本方法灵敏度高、操作简便、结果准确,可用于五味子中五味子醇甲和酯甲定性及定量的测定。

A high performance liquid chromatography-mass spectrometry method was developed for the simultaneous determination of sehisandrin and sehisantherin A in schisandrin mediein and sample preparation 100% methanol solution, and extracted by ultrasonic for 20 rain. The chromatographic conditions are as follows：column of ZORBAXEelipse XDB-C18（ 150 mm × 4.6 mm i. d. ,5 um）eolum,and mobile phase was methanol-water（65：35 ）, flow rate was 0.8 mL/min, wavelength was 220 nm, column temperature was 20 ℃ and the injection volume was 20uL. MS conditions：scanning range was 300 - 600 m/z; temperature of drying gas was 350℃ ; flow rate of drying gas was 8.0 mL/min; pressure of the evaporative gas was 275.8 kPa. The results showed that the standard curves of Sehisandrin and sehisantherin A were linear over the quality range of 1.3 - 83.2 ug and 1.04 - 66.56ug, and the correlation coefficient r were 0. 998 and 0. 997 ,respectively. The average recovery of deoxysehizandrin were 100.7% and 99.7% respectively with RSD less than 2%. The HPLC-LC/MS method was accurate ,rapid, and sensitive. It can be used for the qualitative and quantitative determination of the sehisandrin and sehisantherin A in sehisandra.