摘要
建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定首乌藤中二苯乙烯(二苯乙烯苷、虎杖苷、白藜芦醇)、蒽醌(大黄素、大黄素甲醚、大黄素-8-β-D-葡萄糖苷、芦荟大黄素)、黄酮(表儿茶素、芦丁、金丝桃苷、紫云英苷、槲皮素)及酚酸(没食子酸)等13种成分的方法。采用Waters BEH C18(2.1 mm×100 mm,1.7μm)色谱柱,流动相为水(含0.1%甲酸)-乙腈,梯度洗脱,柱温35℃,流速0.25 m L·min^(-1),采用电喷雾离子源(ESI),多反应离子监测(MRM)扫描方式进行检测。采用TOPSIS法对13种成分进行分析评价。结果 13种成分在一定浓度范围内均呈良好的线性关系,相关系数大于0.991 5,精密度、重复性和稳定性良好;加样回收率在95.24%~102.3%,RSD均小于5%。TOPSIS分析显示广州产的样品综合质量较好。所建立的方法准确、专属性、重复性较好,可用于首乌藤中多元功效物质或指标成分的同时测定,为首乌藤药材内在质量的综合评价和全面控制提供新的方法参考。
A comprehensive analytical method based on UPLC-MS/MS was developed for the simultaneous determination of thirteen components including three stilbenes（ stilbeneglucoside,polydatin,resveratrol）,four anthraquinones（ emodin,physcion,emodin-8-β-D-glucopyranoside,aloe-emodin）,five flavonoids（ epicatechin,rutin,hyperoside,astragalin,quercetin） and one phenolic acid（ gallic acid） in Polygoni Multifori Caulis. The separation was carried out on a Waters BEH C18column（ 2. 1 mm × 100 mm,1. 7 μm）with gradient elution of acetonitrile-water（ 0. 1% acetic acid） at a flow rate of 0. 25 m L·min^-1,and column temperature was 35 ℃.The target compounds were analyzed by multiple reaction monitoring（ MRM） mode. TOPSIS analysis ware performed to evaluate the samples from different areas and commercial herbs according to the contents of thirteen components. The correlation coefficients of all the calibration curves were higher than 0. 991 5. The average recoveries ranged from 95. 24% to 102. 3%,and the relative standard deviations were less than 5%. The result of TOPSIS analysis showed that the comprehensive quality of Polygoni Multifori Caulis sample from Guangzhou was better. The developed method with good repeatability and accuracy was suitable for the simultaneous determination of multiple functional substances,which provided a new basis for the comprehensive assessment and overall control of the quality of Polygoni Multifori Caulis.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2016年第8期1474-1479,共6页
China Journal of Chinese Materia Medica
基金
国家科技支撑计划项目(2011BAI13B04)
江苏高校优势学科建设工程项目(ysxk-2014)
关键词
首乌藤
UPLC-MS/MS
二苯乙烯类
蒽醌
黄酮
酚酸
同时测定
Polygoni Multifori Caulis
UPLC-MS/MS
stilbenes
anthraquinones
flavonoids
phenolic acids
simultaneous determination
