高效液相色谱波长切换法测定不同产地龙胆饮片酒炙前后马钱苷酸与异荭草苷含量  

HPLC determination of loganic acid and isoorientin in Radix Gentiana pieces from different districts before and after wine-processed by wavelength switching

作　　者：马善鹏 吕新 姜宇珺 张北雪 孙建之 才谦 MA Shan-peng;LV Xin;JIANG Yu-jun;ZHANG Bei-xue;SUN Jian-zhi;CAI Qian(Liaoning University of Traditional Chinese Medicine,Dalian Liaoning 116600)

机构地区：[1]辽宁中医药大学药学院

出　　处：《中南药学》2019年第11期1926-1930,共5页Central South Pharmacy

基　　金：辽宁省创新人才支持计划(No.LR2016037)

摘　　要：目的建立同时测定龙胆饮片中活性成分马钱苷酸和异荭草苷含量的HPLC法,并对不同产地龙胆饮片酒炙前后马钱苷酸和异荭草苷的含量差异进行比较,根据含量水平对龙胆药材进行聚类分析。方法色谱柱:Welchrom C18柱(4.6 mm×250 mm,5μm);流动相:0.04%磷酸溶液(A)-甲醇(B),梯度洗脱;流速:1.0 mL·min^-1;检测波长:0~21 min,236 nm(马钱苷酸)、21~25 min,350 nm(异荭草苷);柱温:25℃;进样量:10μL;采用IBM SPSS statistics 24.0软件进行聚类分析。结果马钱苷酸、异荭草苷分别在8.0625~258μg·mL^-1(r=0.9998),0.402~12.85μg·mL^-1(r=0.9997)与峰面积线性关系良好,平均回收率分别为98.8%(RSD=0.94%)、98.2%(RSD=1.2%);聚类分析显示所测龙胆饮片大致分为两类。结论该方法简便准确,分离效果及重复性好,可为龙胆饮片的质量控制提供参考。不同产地龙胆饮片中马钱苷酸和异荭草苷含量存在显著差异,酒炙后两种成分含量大部分呈现下降趋势。Objective To establish an HPLC method for the simultaneous determination of loganic acid and isoorientin,and compare the difference in the two contents in raw and wine-processed Radix Gentiana pieces from different districts.Clustering analysis was used according to the content level.Methods Chromatographic separation was conducted on Welchrom C18 column(4.6 mm×250 mm,5μm)with 0.04%phosphoric acid(A)-methanol(B)as the mobile phase for gradient elution at a flow rate of 1.0 mL·min-1.The wavelength was 236 nm at 21 min to detect loganic acid and switched to 350 nm from 21 to 25 minutes to detect isoorientin.The column temperature was 25℃at the injection volumn of 10μL.Clustering analysis was performed by IBM SPSS statistics 24.0 software.Results There was a good linearity at 8.0625-258μg·mL^-1(r=0.9998)for loganic acid and 0.402-12.85μg·mL^-1(r=0.9997)for isoorientin.The average recoveries were 98.8%(RSD=0.94%)and 98.2%(RSD=1.2%),respectively.Clustering analysis showed that Radix Gentiana pieces were divided into two categories.Conclusion This determination method is accurate and repeatable for the quality control of Radix Gentiana pieces.There is a significant difference in the content of loganic acid and isoorientin in Radix Gentiana pieces from different districts and most decrease after wine-processed.

关 键 词：龙胆饮片 酒炙 马钱苷酸 异荭草苷 高效液相色谱 聚类分析 

分 类 号：R282[医药卫生—中药学] R917[医药卫生—中医学]