摘要
目的:建立UPLC同时测定白术中3种白术内酯成分含量分析方法。方法:样品以甲醇超声提取30 min进行处理。采用超高效液相色谱,以Agilent Poroshell 120 EC-C 18(3.0 mm×150 mm,2.7μm)为色谱柱,流动相水(A)-甲醇(B)梯度洗脱,流速0.5 mL·min^(-1),柱温30℃,检测波长分别为220和276 nm,进样量3μL。采用IBM SPSS 27.0软件对24批白术进行聚类分析和主成分分析。结果:3个成分在考察的浓度范围内,浓度与峰面积之间呈良好的线性关系(r>0.999),回收率均在103.05%~106.35%,RSD 2.0%~3.3%。经聚类分析发现,24批白术药材可聚为四大类;经主成分分析发现,2个主成分因子的累计方差贡献率为98.975%(第一主成分、第二主成分的贡献率分别为92.124%、6.601%)。结论:该方法简便、快捷、准确且灵敏度高,对评控白术药材的质量提供参考。
Objective:To establish a UPLC method for the simultaneous determination of three atractylenolides in Atractylodes macrocephala.Methods:The samples were extracted with methanol for 30 min by ultrasonic method.Three compounds in A.macrocephala were simultaneously determined by UPLC with Agilent Poroshell 120 EC-C 18(3.0 mm×150 mm,2.7μm),with water(A)-methanol(B)as the mobile phase for gradient elution;at the flow rate of 0.5 mL·min^(-1);the determination wavelength was 220 and 276 nm;and the injection volume was 3μL.Cluster analysis and principal component analysis were performed by IBM SPSS 27.0 statistical software.Results:There was a good linear relationship between the concentration and peak area of all the three components in the investigated concentration range(r>0.999).The average recoveries ranged from 103.05%to 106.35%with RSD of 2.0%-3.3%.Through cluster analysis,24 batches of A.macrocephala could be clustered into 4 groups.According to the principal component analysis,the cumulative variance contribution rate of the two principal component factors was 98.975%(contribution rates of first principal components and second principal components were 92.124%and 6.601%).Conclusion:The method is simple,rapid,accurate and highly sensitive to provide a reference for quality evaluation of A.macrocephala.
作者
周海艳
高云佳
王敏
张庆英
屠鹏飞
ZHOU Haiyan;GAO Yunjia;WANG Min;ZHANG Qingying;TU Pengfei(State Key Laboratory of Natural and Biomimetic Drugs,School of Pharmaceutical Sciences,Peking University,Beijing 100191,China;SinoPharm Pharmaceuticals Limited,Beijing 102206,China)
出处
《中国药品标准》
CAS
2023年第1期5-14,共10页
Drug Standards of China
基金
国家重点研发计划(2018YFC1707904,2018YFC1707900)。
关键词
白术
白术内酯Ⅲ
白术内酯Ⅱ
白术内酯Ⅰ
超高效液相色谱
聚类分析
主成分分析
Atractylodes macrocephala
atractylenolideⅢ
atractylenolideⅡ
atractylenolideⅠ
UPLC
cluster analysis
principal component analysis
