柱前衍生化高效液相色谱法测定伊贝母中西贝素的含量

Analysis of sipeimine in Bulbus Fritillariae pallidiflorae by HPLC after derivatization

目的：采用柱前衍生化反相高效液相色谱法测定中药伊贝母中西贝素的含量。方法：色谱柱为ＯＤＳ柱，流动相为甲醇水（９０∶１０），内含４ｍｌ·Ｌ－１的三乙胺，检测波长２２７ｎｍ。结果：西贝素苯甲酸酯的峰面积与该生物碱的重量在０．４～３．５μｇ范围内呈良好的线性关系，回归方程为Ｙ＝－２．０４×１０３＋６．０６×１０４Ｘ，ｒ＝０．９９９６；平均回收率为１０１．０％（ｎ＝５，ＲＳＤ＝２．８％）。结论：西贝素为伊贝母中主要生物碱成分。

OBJECTIVE: A new method was developed for the determination of sipeimine in Bulbus Fritillariae pallidiflorae by HPLC after derivatization with benzoyl chloride. METHODS: The chromatographic system consisted of an ODS column and a mobile phase of methanol water (90∶10) containing 4 ml·L -1 triethylamine. The detector was set to 227 nm to monitor the derivative benzoate ester. RESULTS: Under the derivatization conditions optimized, the calibration curve was Y=-2.04×10 3+6.06×10 4X, r=0.999 6 for sipeimine, where Y was the peak area and X was the weight of sipeimine; average recovery was 101.0% (n=5, RSD=2.8%). CONCLUSION: The results show that sipeimine is the major component in alkaloids from Bulbus Fritillariae pallidiflorae.