基于UPLC特征图谱和多指标含量测定南五味子质量控制

Quality Control of Schisandra Chinensis from Different Production Area Based on UPLC Characteristic Chromatogram and Multi-index Content Determination

目的:建立南五味子UPLC特征图谱方法,并同时测定不同产地药材中五味子甲素、安五脂素和五味子酯甲含量,为其质量控制及评价提供参考。方法:采用ACQUITY BEH C_(18)(150 mm×2.1 mm,1.7μm)色谱柱,以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱,检测波长为280 nm,12 min切换至220 nm,柱温为35℃,流速为0.3 mL/min,测定不同产地的15批南五味子特征图谱及含量,运用聚类分析法比较不同产地、不同批次间南五味子质量差异。结果:确定15批南五味子UPLC特征图谱中10个共有特征峰,并指认了5‐羟甲基糠醛、原儿茶酸、五味子酯丙、五味子酯甲、五味子酯乙、五味子酯丁、安五脂素和五味子甲素8个成分。五味子酯甲、安五脂素、五味子甲素的进样量分别在0.0085~1.5388μg、0.0246~3.1944μg、0.0216~2.7705μg范围内线性关系良好,加样回收率分别为99.42%、99.36%、98.37%;五味子甲素、安五脂素和五味子酯甲精密度、稳定性、重复性试验的RSD均小于2.0%。结论:所建立的方法准确、简便、重现性良好,可用于南五味子的质量控制,分析结果显示五味子酯甲含量在陕西省西安市周至县、山西省运城市平陆县产区含量较高,相较其他产区具备显著差异;安五脂素含量在陕西省安康市旬阳县,四川省绵阳市平武县产区含量较高,相较陕西西安周至县具备显著差异;五味子甲素含量在不同产区、相同产地不同批次间存在一定波动,各产区之间无显著差异。

Objective Establish UPLC characteristic method for Schisandra chinensis and determine the content of schizandrin A,anwuligan and schisantherin A,provide reference for its quality control and evaluation.Methods An ACQUITY BEH C_(18)(150 mm×2.1 mm,1.7μm)column was used for gradient elution with acetonitrile-0.1%phosphoric acid solution as mobile phase.Detection wavelength:at 280 nm and switch to 220 nm after 12 minutes,the column temperature was 35℃and the flow rate was 0.3 mL per minute.The characteristic map and content of 15 batches of S.chinensis from different producing areas were determined.Cluster analysis was used to compare the quality difference of S.chinensis from different producing areas and different batches.Results Ten common characteristic peaks were identified in 15 batches of UPLC characteristic maps of SCHisandrae chinensis,and eightcompounds of 5-hydroxymethylfurfural、protocatechuic acid、schisantherin C、schisantherin A、schisantherin B、schisantherin Danwuligan and schizandrin A wereidentified by Reference Substances.The linear ranges of schisantherin A、anwuligan and schisandrin A were 0.0085~1.5388μg,0.0246-3.1944μg,0.0216-2.7705μg,and the recoveries were 99.42%,99.36%,98.37%,respectively.RSDS of precision,stability and repeatability tests of schisandrin a,andpentalipoid and schisandrin ester a were all less than 2.0%.Conclusion The established method is accurate,simple and reproducible,and can be used for the quality control of SCHisandra chinensis.The results showed that the content of schisantherin A was higher in Pinglu,Shanxi Province and Zhouzhi,Shaanxi Province.And significantly different from other producing areas.The content of anwuligan is higher in Xunyang County,Shaanxi Province and Pingwu,Sichuan Province.And significantly different from Zhouzhi,Shaanxi Province.The content of schisandrin in different producing areas and different batches of the same producing area fluctuated to some extent,but there was no significant difference among producing areas.