摘要
目的建立同时测定双五胶囊中紫丁香苷、五味子醇甲、五味子甲素、五味子乙素含量的方法。方法HPLC法,采用Diamonsil C18柱(200mm×4.6mm,5μm),流动相为A:甲醇-乙腈(1∶1),B:水,梯度洗脱,0～5min,35%～60%A;5～10min,60%～70%A;10～50min,70%～90%A;50～90min,90%A。流速为1ml/min,柱温:35℃,检测波长220nm。结果紫丁香苷、五味子醇甲、五味子甲素、五味子乙素浓度分别在1.28～20.40μg/ml(r=0.9997)、6.30～100.80μg/ml(r=0.9996)、1.20～19.20μg/ml(r=0.9998)和3.75～60.00μg/ml(r=0.9996)范围内呈良好的线性关系。4种成分精密度实验RSD<1%。24h内稳定性RSD<1.5%。紫丁香苷、五味子醇甲、五味子甲素、五味子乙素的平均加样回收率分别为99.47%、102.50%、99.21%、101.86%。结论所建立的方法具有快速、简便、准确等优点,可用于双五胶囊的质量控制。
Objective To establish an HPLC method for simultaneous determination of syringin,schizandrin,deoxyschizandrin and schisandrin B in Shuangwu capsules. Methods The HPLC method was employed using a Diamonsil C18 column （ 200 mm × 4. 6 mm,5 μm） with a mobile phase of methanol-acetonitrile （ 1∶ 1,A） and water （ B）. The gradient elution program was as follows：0-5 min,35% -60% A; 5-10 min,60%-70% A; 10-50 min,70% -90% A; 50-90 min,90% A. The flow rate was 1 ml/min. The detection wavelength was set at 220 nm and the temperature was at 35℃. Results The linearity was obtained within the range of 1. 28 -20. 40 μg/ml for syringin （ r = 0. 999 7） ,6. 30-100. 80 μg/ml for schisantherin （ r = 0. 999 6） ,1. 20-19. 20 μg/ml for deoxyschi-zandrin （ r = 0. 999 8） ,and 3. 75-60. 00 μg/ml for schisandrin B （ r = 0. 999 6）. The RSD values of precision were less than 1% for all the four components. The results showed that the samples were stable in the room temperature for at least 24 h. The average recovery. rates of syringin,schizandrin,deoxyschizandrin and schisandrin B were 99. 47% ,102. 50% ,99. 21% and 101. 86% ,respectively. Con-clusion Our method is rapid,easy to perform and accurate; it can be used to control the quality of Shuangwu capsules.
出处
《第二军医大学学报》
CAS
CSCD
北大核心
2010年第1期91-93,共3页
Academic Journal of Second Military Medical University
