HPLC-ELSD法测定白头翁总皂苷碱水解产物中8种皂苷  

Simultaneous determination of eight saponins in alkali hydrolysate of total saponins from Pulsatilla chinensis by HPLC-ELSD

作　　者：季秀美[1] 舒展[1] 许琼明[1] 刘艳丽[1] 杨世林[1] 

机构地区：[1]苏州大学药学院,江苏苏州215123

出　　处：《中草药》2013年第11期1416-1419,共4页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(81273402);重大新药创制国家科技重大专项资助(2011ZX11102);江苏省自然科学基金(BK2012620)

摘　　要：目的建立同时测定白头翁总皂苷碱水解产物中8种皂苷成分的HPLC-ELSD方法。方法采用Kromasil C18色谱柱(250 mm×4.6 mm,5μm);流动相为甲醇-0.2%甲酸水溶液;柱温35℃;梯度洗脱条件:0～30 min,70%～100%甲醇;体积流量1.0 mL/min;ELSD气化室温度40℃;气体压力350 kPa。结果白头翁皂苷D、常春藤皂苷元3-O-β-D-吡喃葡萄糖基-(1→4)-α-L-吡喃阿拉伯糖、白头翁皂苷A、黑海常春藤苷A1、白头翁皂苷F、齐墩果酸3-O-β-D-吡喃葡萄糖基-(1→4)-β-D-吡喃葡萄糖基-(1→3)-α-L-吡喃鼠李糖基-(1→2)-α-L-吡喃阿拉伯糖苷、齐墩果酸3-O-β-D-吡喃葡萄糖基-(1→3)-α-L-吡喃鼠李糖基-(1→2)-α-L-吡喃阿拉伯糖苷、齐墩果酸3-O-α-L-吡喃鼠李糖基-(1→2)-α-L-吡喃阿拉伯糖苷进样量分别在0.799～4.568、0.563～6.756、0.431～2.683、0.894～7.826、0.643～7.504、1.351～7.822、0.629～2.515、0.698～2.794μg,峰面积(A)的对数值lgA与相应质量(M,μg)的对数值lgM呈良好的线性关系(n=5),8种成分的平均回收率在99.0%～101.0%,且RSD值均小于1.5%。结论本检测方法简便、准确,为白头翁总皂苷碱水解产物的质量控制提供了依据。Objective To develop an HPLC method for the simultaneous determination of eight saponins in alkali hydrolysate of total saponins from Pulsatilla chinensis. Methods HPLC was performed on a Kromasil C18 analytical column （250 mm × 4.6 mm, 5.0 μm） at 35 ℃ with MeOH-0.2% HCOOH solution as the mobile phase by gradient elution and the step gradients were as follows： 0--30 min, 70%--100% MeOH; The flow rate was 1.0 mL/min; ELSD gasification chamber temperature was 40 ℃; Gas pressure of carrier gas N2 was 350 kPa. Results The linear response （the log values of peak areas with corresponding log values of sample introducing amounts） ranges were 0.799--4.568 μg for pulsatilla saponin D, 0.563--6.756μtg for hederagenin 3-O-β-D-glucopyranosyl-（1→4）-α-L- arabinopyranoside, 0.431--2.683 μg for pulsatilla saponin A, 0.894-7.826 μg for hederacolchiside A1, 0.643--7.504 μg for pulsatilla saponin F, 1.351--7.822μg for oleanolic acid 3-O-β-D-glucopyransyl-（1→4）-β-D-glucopyransyl（1→3）-α-L-rhamnrmpyranosyl- （1→2）-α-L-arabinopyranoside, 0.629--2.515 μg for oleanolic acid 3-O-β-D-glucopyranosyl-（1→3）-α-L-rhamnopyranosyl- （1→2）-α-L-arabinopyranoside, and 0.698--2.794 μg for oleanolic acid 3-O-α-L-rhamnopyranosyl-（1→2）-α-L-arabinopyranoside, respectively （n = 5）. The average recoveries of the eight saponins were between 99.0% and 10i.0%, and RSD values were less than 1.5%. Conclusion The results demonstrate that the established method has the adequate accuracy and selectivity for the quality control of alkali hydrolysate of total saponins from P. chinensis.

关 键 词：白头翁总皂苷碱水解产物 HPLC-ELSD 白头翁皂苷D 白头翁皂苷A 黑海常春藤苷A1 白头翁皂苷F 

分 类 号：R286.02[医药卫生—中药学]