摘要:
目的: 建立同时测定总状土木香药材中3个倍半萜类同分异构体的高效液相方法。 方法: 采用Agilent ZorbaxXDB-C18 column(250 mm×4.6 mm,5μm);流动相:55%乙腈和45%水等度洗脱;流速1ml/min;检测波长210 nm。 结果: 总状土木香药材中3个倍半萜类同分异构体Igalane、异土木香内酯和土木香内酯分别在17.40～1 740.00、21.20～2 120.00和20.40～2 040.00μg/ml的浓度范围内呈良好的线性关系,最低检测限分别为0.087、0.042和0.041μg/ml。重复性、稳定性的RSD均小于2.85%;各成分平均回收率均小于104.43%,RSD<1.20%。 结论:该方法>快速简便、准确可靠,各主要化学成分均能达到基线分离,适用于总状土木香药材的质量控制。另外,本实验采用液相半制备得到了两个倍半萜类同分异构体,并对它们的结构进行了鉴定。
Abstract:
Objective To establish a method of HPLC for the simultaneous quantification of three sesquiterpene lactones in Inula racemosa. Methods Agilent Zorbax XDB-C18 column(250 mm×4.6 mm,5 μm) was uesed with a mobile phase consists of 55% acetonitrile and 45% water,at a flow rate of 1.0 ml/min,and detection wavelength of 210 nm. Results Three sesquiterpene lactones in Inula racemosa Hook.f.,namely igalane(1),isoalantolactone(2) and alantolactone(3) has good linear relation in 17.40～1 740.00,21.20～2 120.00,20.40～2 040.00 μg/ml with the lowest detection limit of 0.087,0.042,0.041 μg/ml respectively.The RSD of repeatability and stability were all less than 2.85%.The average recovery rate of there constituents were all less than 104.43% with RSD less than<1.20%. Conclusion The method was rapid,accurate,reliable and could be suitable as a quality control method for I.racemosa.Two minor isomers from I.racemosa were isolated by semi-preparative HPLC which structures were elucidated on the basis of NMR analysis.
点击查看大图
下载:
