摘要
目的 :采用高效液相色谱法 -蒸发激光散射检测器测定银杏酮酯舌下片中总内酯的含量 ,以控制该制剂质量。方法 :应用高效液相色谱 -蒸发激光散射检测法分析 4种萜类内酯的含量。色谱条件为 :Diamonsil TM (钻石 ) C1 8色谱柱(2 5 0 mm× 4 .6 mm,5μm) ;流动相 :甲醇 -水 (36 :6 4 ) ;柱温 :30 o C;流速为 0 .6 ml/ min;检测器条件 :漂移管温度为 4 0 o C,载气压力为 2 .0 bar,灵敏度为 6。结果 :4种萜类内酯之间分离度均达 2 .5以上 ;理论板数以白果内酯峰计算为 830 8,6次平均加样回收率分别为 :白果内酯 10 2 .3% (RSD为 1.4 9% ) ,银杏内酯 C 10 2 .6 % (RSD为 1.31% ) ,银杏内酯 A 10 1.2 % (RSD为 2 .39% ) ,银杏内酯 B98.0 % (RSD为 2 .75 % ) ;白果内酯、银杏内酯 C、银杏内酯 A、银杏内酯 B,分别在 3.4～ 2 0 .4 μg、2 .2 2～ 13.32μg、2 .4 6～ 14 .76μg、2 .0 6～ 12 .36μg范围内 ,进样量对数值与峰面积对数值呈良好的线性关系。结论 :本法测定银杏酮酯舌下片中萜类内酯的含量 ,结果准确 。
Object: To determine the content of Tieleineizhi of Yinxingtongzhi sublingual with HPLC-ELSD for the quality control of the product. Methods: The separation was performed on a Diamonsil C18 column (150mm×4.6mm ID, 5μm).The mobile phase consists of methanol-water (36:64) at a flow rate of 0.6mL/min. An evaporative light-scattering detector (ELSD) Model SEDEX 75 (DIKMA France) was used. The parameters was set as follows: drift tube temperature was 30℃, the pressure of carrier gas was 2.0 bar and gain was 6. Results: The separation degrees of four Tieleineizhi were all above 2.5. The number of theoretical plates calculated on Ginkgolide peak was 8308. The average recovery of the added were 102.3% (RSD 1.49%) for Ginkgolide, 102.6% (RSD 1.31%) for Ginkgolide C, 101.2%(RSD 239%) for Ginkgolide A and 98.0%(RSD 2.75%) for Ginkgolide B , respectively. There were good linear relationship between the log values of the inject quantities and the peak areas over the range of 3.4～20.4μg for Ginkgolide, 2.22～13.32μg for Ginkgolide C, 2.46～14.76μg for Ginkgolide A and 2.06～12.36μg for Ginkgolide B , respectively. Conclusion: The method was highly reproducible and accurate.
出处
《天津药学》
2003年第6期9-11,共3页
Tianjin Pharmacy
