HPLC-ELSD法测定心脑苏滴丸中银杏内酯含量

Determination of Ginkgolides in Xinnaosu Dropping Pills by HPLC-ELSD

目的建立高效液相色谱-蒸发光散射检测(HPLC-ELSD)法测定心脑苏滴丸中的银杏内酯(白果内酯、银杏内酯A、银杏内酯B和银杏内酯C)的含量。方法采用十八烷基硅烷键合硅胶色谱柱(Thermo,Hypersil 250 mm×4.6 mm,5μm),以正丙醇-水(1∶84,V/V)混合液(A)和四氢呋喃(B)为流动相,柱温35℃,流动相流速1 mL·min^(-1),漂移管温度为50℃,气体流量为1.2 L·min^(-1)。结果 HPLC-ELSD法可同时测定的白果内酯、银杏内酯A、银杏内酯B和银杏内酯C,白果内酯在0.0434～0.136 mg·mL^(-1)浓度范围内,银杏内酯A在0.734～1.835 mg·mL^(-1)浓度范围内,银杏内酯B在0.366～0.915 mg·mL^(-1)浓度范围内,银杏内酯C在0.417～1.336 mg·mL^(-1)浓度范围内分别呈良好的线性关系。结论本方法灵敏度高,准确性强,适用于测定心脑苏滴丸中的白果内酯、银杏内酯A、银杏内酯B和银杏内酯C含量。

OBJECTIVE To establish the method to determine the content of ginkgolides( bilobalide,ginkgolide A,ginkgolide B and ginkgolide C) in Xinnaosu dropping pills by HPLC-ELSD. METHODS A HPLC-ELSD method was set. Thermo C18( 250 mm×4.6 mm,5 μm) was used.The Normal propyl alcohol was mixed with water in 1 ∶84 as mobile phase A and tetrahydrofuran as mobile phase B.The column temperature was set at 35 ℃.The flow rate was 1.0 m L·min^-1.The tube temperature of the detertor was 50 ℃.The gain flow rate was 1.2 L·min^-1. RESULTS The bilobalide,ginkgolide A,ginkgolide B and ginkgolide C were determined by HPLC-ELSD. The bilobalide,ginkgolide A,ginkgolide B and ginkgolide C were linear at the range of 0.0434-0.136 mg·mL^-1,0.734-1.835 mg·mL^-1,0.366-0.915 mg·mL^-1 and 0.417-1.336 mg·mL^-1 respectively. The average recovery were from 95% to 105%. CONCLUSION This method is sensitive and accurate for the determination of bilobalide,ginkgolide A,ginkgolide B and ginkgolide C in Xinnaosu dropping pills.