摘要
目的:研究四制香附的质量评价方法。方法:建立香附和四制香附的超高效液相色谱法(UPLC)指纹图谱并通过化学计量学方法比较炮制前后指纹图谱中总体化学成分的变化,流动相甲醇(A)-水(B)梯度洗脱(0~10 min,5%~40%A;10~30 min,40%~70%A;30~40 min,70%A),流速0.3 mL·min^(-1),进样量3μL,柱温35℃,检测波长280 nm。采用UPLC比较香附四制前后主要指标成分香附烯酮和α-香附酮的含量变化,流动相甲醇-水(75∶25),检测波长242 nm。结果:四制对香附指纹图谱中化学成分的总体特征产生了显著影响。香附和四制香附的指纹图谱中共标示了28个特征峰,其中峰1,2,4为四制香附的特有峰,峰5为香附的特有峰,经指认峰2为5-羟甲基糠醛,峰24为香附烯酮,峰27为α-香附酮。香附四制后产生的5-羟甲基糠醛来源于四制辅料中的米醋、黄酒及香附中多糖类成分的美拉德反应。定量分析结果显示,四制前后香附烯酮含量差异无统计学意义,但α-香附酮含量明显降低。结论:香附四制过程中存在结构转化产生新成分且伴随着指标成分含量变化,可作为区别香附和四制香附的专属特征标识和差异性特征标识。该研究从定性和定量2个方面快速有效地评价了香附和四制香附,建立的方法准确性强、稳定性好,为完善香附和四制香附的质量评价体系提供了实验依据。
Objective: To study the quality evaluation method of Cyperi Rhizoma processed with four excipients. Method: Ultra-performance liquid chromatography(UPLC) fingerprints of raw products and processed products with four excipients of Cyperi Rhizoma were established,and the changes of chemical components in the fingerprints before and after processing were compared by chemometric analysis. The mobile phase was consisted of methanol(A)-water(B)for gradient elution(0-10 min,5%-40%A;10-30 min,40%-70%A;30-40 min,70%A)at a flow rate of 0.3 mL·min^(-1). The injection volume was 3 μL,the column temperature was 35 ℃, and the detection wavelength was 280 nm. The content changes of main index components in Cyperi Rhizoma before and after processing were compared by UPLC. The mobile phase was methanol-water(75∶25)and the detection wavelength was 242 nm. Result: Processing with four excipients had a significant impact on the overall characteristics of chemical components in the fingerprint of Cyperi Rhizoma. A total of 28 characteristic peaks were identified in fingerprints of the raw and processed products. Among them,peaks 1,2 and 4 were specific peaks of the processed products,peak 5 was characteristic peak of the raw products. Peak 2 was identified as 5-hydroxymethylfurfural,peak 24 as cyperenone and peak 27 as α-cyperone.The 5-hydroxymethylfurfural produced by the processing with four excipients came from rice vinegar,rice wine and Maillard reaction of polysaccharides in Cyperi Rhizoma. The results of determination showed that there was no significant difference in the content of cyperenone after processing,but the content of α-cyperone decreased significantly. Conclusion: In the process of Cyperi Rhizoma processed with four excipients,there are new components produced by structural transformation,which are accompanied by changes in the content of index components. In this study,the quality of raw and processed products of Cyperi Rhizoma can be rapidly and effectively evaluated from qualitative and quantitative aspects.
作者
刘聪
王丽霞
杨晓芸
陈晓旭
蒋彤
唐力英
张琼
王祝举
LIU Cong;WANG Li-xia;YANG Xiao-yun;CHEN Xiao-xu;JIANG Tong;TANG Li-ying;ZHANG Qiong;WANG Zhu-ju(School of Pharmacy,Shanxi Medical University,Taiyuan 030001,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2021年第15期76-82,共7页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家重点研发计划项目(2018YFC1707106)。
关键词
四制香附
美拉德反应
指纹图谱
炮制
香附烯酮
Α-香附酮
超高效液相色谱法(UPLC)
Cyperi Rhizoma processed with four excipients
Maillard reaction
fingerprint
processing
cyperenone
α-cyperone
ultra-performance liquid chromatography(UPLC)
作者简介
第一作者:刘聪,在读硕士,从事饮片化学成分及炮制原理研究,E-mail:wanlc919919@163.com;通信作者:唐力英,副研究员,从事饮片化学成分及炮制原理研究,E-mail:bjtangliying@163.com;通信作者:张琼,教授,从事天然产物研究,E-mail:zhangqiong_83@hotmail.com。
