九蒸九晒炮制过程何首乌中5-羟甲基糠醛和二苯乙烯苷含量变化分析  

Changes of content of 5-HMF and stilbene glycoside in Polygoni Multiflori Radix during nine-time repeat of steaming and sun-drying

作　　者：王莹[1] 辜冬琳 范晶 杨建波[1] 刘越[3] 王雪婷 汪祺[1] 金红宇[1] 魏锋[1] 马双成[1] WANG Ying;GU Donglin;FAN Jing;YANG Jianbo;LIU Yue;WANG Xueting;WANG Qi;JIN Hongyu;WEI Feng;MA Shuangcheng(National Institutes for Food and Drug Control,Beijing 100050,China;China Pharmaceutical University,Nanjing Jiangsu 210009,China;Beijing University of Chinese Medicine,Beijing 100029,China)

机构地区：[1]中国食品药品检定研究院,北京100050 [2]中国药科大学,江苏南京210009 [3]北京中医药大学,北京100029

出　　处：《中国药物警戒》2022年第12期1291-1294,1308,共5页Chinese Journal of Pharmacovigilance

基　　金：国家自然科学基金资助项目(81973476);国家自然科学基金资助项目(81903807)。

摘　　要：目的探索何首乌炮制过程中5-羟甲基糠醛(5-HMF)和二苯乙烯苷含量变化规律,为何首乌质量评价提供参考。方法九蒸九晒法炮制何首乌,采用Agilent SB-C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇-水(8∶92)为流动相等度洗脱,流速为1.0 mL·min^(-1),检测波长为280 nm,柱温为30℃,测定样品中5-HMF的含量;按照《中华人民共和国药典》(2020版)中何首乌项下方法,测定炮制过程中何首乌中二苯乙烯苷含量。结果建立的何首乌中5-HMF含量测定方法,通过方法学验证试验证明其符合样品测定要求。5-HMF在生品中未检出,随着炮制次数的不断增加,5-HMF含量呈逐渐上升趋势;同时随着炮制次数的增加,二苯乙烯苷含量总体呈下降趋势。结论在炮制过程中,何首乌中5-HMF和二苯乙烯苷含量发生显著变化,本研究可为何首乌炮制机理研究及其质量评价方法的完善提供重要参考。Objective To explore the changes of contents of 5-hydroxymethylfurfural(5-HMF)and stilbene glycoside in Polygoni Multiflori Radix(PM)during nine-time repeat of steaming and sun-drying and to provide reference for quality evaluation of PM.Methods The samples were prepared using the nine-time repeat of steaming and sun-drying method.The contents of 5-HMF were determined on an Agilent SB-C_(18)(4.6 mm×250 mm,5μm)column with a mobile phase composed of methanol and water solution(8:92)at a flow rate of 1.0 mL·min^(-1)and at the column temperature of 30℃.The contents of stilbene glycoside were determined using the method for PM specified in Chinese Pharmacopoeia(2020 Edition).Results The established method for the determination of 5-HMF in PM proved to meet the requirements of sample determination according to methodological validation tests.5-HMF was not detected in the raw PM.The content of 5-HMF increased gradually with the number to times of processing,but the content of stilbene glycoside from PM trended down.Conclusion In the process of nine-time repeat of the steaming and sun-drying,the contents of 5-HMF and stilbene glycoside from PM can change significantly.This study can provide reference for the study on the processing mechanism of PM and for improvement of quality evaluation methods.

关 键 词：何首乌 九蒸九晒 质量评价 二苯乙烯苷 5-羟甲基糠醛 

分 类 号：R927.2[医药卫生—药学]