HPLC-QAMS法测定不同产地19批山茱萸中5种环烯醚萜苷类成分的含量

Content Determination of 5 Iridoid Glycosides in 19 Batches of Corni Fructus from Different Origins by HPLC-QAMS Method Simultaneously

目的:测定不同产地19批山茱萸中5种环烯醚萜苷类成分的含量。方法:采用高效液相色谱(HPLC)-一测多评(QAMS)法。色谱柱为Agilent XDB-C_(18),流动相为甲醇-水,梯度洗脱,流速为1.0 m L/min,柱温为35℃,进样量为15μL,检测波长为240nm。以山茱萸中的马钱苷为内参物,建立其与山茱萸中另外4种环烯醚萜苷类成分即莫诺苷、当药苷、山茱萸苷和山茱萸裂苷之间的相对校正因子并进行适用性评价后计算4种成分的含量;另采用HPLC-外标法测定19批药材中上述5种成分的含量,比较两种方法测定结果的差异,验证QAMS法的准确性。结果:在适用性评价中,不同试验条件下4种成分的相对校正因子的RSD均小于2%;两种测定方法下,4种成分的含量比较差异均无统计学意义(P均大于0.05)。结论:本研究建立的HPLC-QAMS法可用于山茱萸中5种环烯醚萜苷类成分的含量测定,且方法准确、可靠、快速,成本更低。

OBJECTIVE:To determine the contents of 5 iridoid glycosides in 19 batches of Corni fructus from different origins.METHODS:HPLC-QAMS method was adopted.The determination was performed on Agilent XDB-C18 column with mobile phase consisted of methanol-water(gradient elution)at the flow rate of 1.0 mL/min.The column temperature was set at 35℃,and sample size was 15μL.The detection wavelength was set at 240 nm.Using loganin in Corni fructus as internal standard,relative correction factors(RCF)of loganin to other 4 iridoid glycosides as monod glycosides,officinosides,cornus glucosides and cornus glucosides were established.The contents of 4 kinds of components were calculated after suitability evaluation.The contents of 5 kinds of components in 19 batches of samples were determined by HPLC external standard method.The differences of two methods were compared;the accuracy of QAMS was validated.RESULTS:RSDs of RCF for 4 components under different trial conditions were all lower than 2%in suitability evaluation.P value of content comparison of 4 components between 2 methods were all higher than 0.05.CONCLUSIONS:HPLC-QAMS method can be used for content determination of 5 iridoid glycoside in Corni fructus.It is accurate,reliable,rapid and less costly.