摘要
目的建立UPLC-MS分析技术同时测定不同产地制何首乌饮片中4种蒽醌类(大黄素甲醚、大黄素、大黄素甲醚-8-O-β-D-葡萄糖苷和大黄素-8-O-β-D-葡萄糖苷)及3种鞣质类(没食子酸、儿茶素、表儿茶素)和1种二苯乙烯类(反式二苯乙烯苷)活性成分的含量。方法采用Ultimate UPLC-XB C18(2.1 mm×50 mm,1.7μm)色谱柱,流动相A为0.1%甲酸水溶液,流动相B为乙腈,线性梯度洗脱,流速为0.2 mL·min^(-1);采用电喷雾离子源(ESI)、负离子扫描模式,在多反应监测(MRM)条件下进行定量分析;并用IBM SPSS Statistics 22软件对数据结果进行聚类分析。结果建立的UPLC-MS可以较好地分离8种成分,各成分在相应浓度范围内与峰面积线性关系良好;其定量限和检测限范围分别为0.89~13.00和0.20~4.00 ng·mL^(-1);精密度、重复性、稳定性的RSD值(n=5)均小于5%;加样回收率在99.47%~101.49%,RSD均小于2.5%;聚类分析结果显示12批制何首乌样品分为3类,其中S1、S2、S5、S8~S12归为Ⅰ类,S6、S7归为Ⅱ类,S3和S4归为Ⅲ类;第Ⅲ类样本(广西、广东)中3类成分的平均含量相对较高。结论该方法可靠、准确、快速、重复性好,可用于制何首乌的质量控制与品质相关研究,并为其临床安全用药提供依据。
Objective To determine 4 anthraquinones(physcion,emodin,physcion-8-O-β-Dglucoside and emodin-8-O-β-D-glucoside),3 tannins(gallic acid,catechin,and epicatechin)and 1 stilbene glycoside(trans-THSG)in Polygonum multiflorum decoction slices from different regions by UPLC-MS.Methods Ultimate UPLC-XB C18(2.1 mm×50 mm,1.7μm)column was used with 0.1%formic acid as mobile phase A and acetonitrile as mobile phase B.Linear gradient elution was performed at the flow rate of 0.2 mL·min^(-1).Quantitative analysis was performed with ESI source,negative ion scanning mode and multi-reaction monitoring(MRM).IBM SPSS Statistics 22 was used for cluster analysis.Results The UPLC-MS method well separated the 8 target components with good linearity in the corresponding concentration ranges.The limits of quantification and detection were 0.89~13.00 and 0.20~4.00 ng·mL^(-1),respectively.RSDs of precision,repeatability and stability(n=5)were all less than 5%.The recoveries ranged from 99.47%to 101.49%,and RSDs were all lower than 2.5%.Cluster analysis showed that the 12 batches of Polygonum multiflorum samples were divided into 3 categories,among which S1,S2,S5,S8~S12 were classified as classⅠ,S6 and S7 classified as classⅡ,while S3 and S4 classified as classⅢ.The average content of 3 components in classⅢsamples from Guangxi and Guangdong was relatively high.Conclusion The method is reliable,accurate,rapid and reproducible.It can be used to determine the content of 8 components in Polygonum multiflorum from different regions,and provide reference for the quality control of Polygonum multiflorum,as well as for safety and quality research.
作者
刘野
武俊颖
贺奥城
杨武亮
张武岗
陈海芳
LIU Ye;WU Jun-ying;HE Ao-cheng;YANG Wu-liang;ZHANG Wu-gang;CHEN Hai-fang(Key Laboratory of Modern Preparation of Traditional Chinese Medicine,Ministry of Education,Jiangxi University of Chinese Medicine,Nanchang 330004;National Engineering Research Center for Manufacturing Technology of Solid Chinese Medicine Preparations,Jiangxi University of Chinese Medicine,Nanchang 330004;Jiangxi Bencao Tiangong Technology Co.,Ltd.,Nanchang 330006)
出处
《中南药学》
2023年第6期1634-1639,共6页
Central South Pharmacy
基金
国家自然科学基金项目(No.81903917,No.81660650)
江西省教育厅项目(No.GJJ190671,No.GJJ170723)
江西省中医药中青年骨干人才培养计划(No.S21-09)
江西中医药大学博士科研启动基金(No.2018WBZR002)。
