首页|基于波长转换RP-HPLC法的茯苓皮多成分含量测定及特征图谱方法研究

基于波长转换RP-HPLC法的茯苓皮多成分含量测定及特征图谱方法研究

扫码查看
目的:本文通过建立茯苓皮的双波长切换HPLC特征图谱方法 ,同时建立茯苓皮中11个三萜类成分含量的测定方法,旨在为茯苓皮全面的质量评价提供定性和定量方法.方法:采用Agilent5 HC-C18(2)色谱柱(250 mm ×4.6 mm,5 μm),流动相为乙腈(含3%四氢呋喃)(A)和0.1%磷酸水溶液(B),梯度洗脱,流速1 mL·min-1,柱温35 ℃,进样体积20μL,检测波长210、243 nm.结果:所建立的特征图谱能有效的识别18个共有峰,精密度、重复性、稳定性(48 h)试验的RSD均<3.7%(n=6);11个待测化学成分能够达到良好分离,在考察质量范围内线性关系良好(r均≥ 0.999 6),平均回收率95.4%~105.5%,RSD 1.0%~3.1%,精密度、重复性、稳定性(48 h)试验的RSD均≤3.0%(n=6);相似度分析结果显示,大部分产地的茯苓皮药材的相似度很高;含量测定结果表明,11个三萜类成分中茯苓酸A在所有批次茯苓皮中占比最高,另外茯苓酸A、松苓新酸、茯苓酸B、去氢齿孔酸、栓菌酸5个成分的含量波动相对较大,其他成分波动较平缓;不同产地茯苓皮样品无明显地域上的差异.结论:建立了茯苓皮特征图谱和多成分含量测定方法,为茯苓皮的质量控制奠定了基础.
Determination and characterization of Poriae Cutis multi-component content based on wavelength conversion RP-HPLC method
Objective:To comprehensively evaluate the quality of Poriae Cutis,and to establish a dual wavelength switching HPLC method for comparing the characteristic spectra of Poriae Cutis and studying the content of 11 triterpenoid components,to provide reference for the qualitative and quantitative research of Poriae Cutis.Methods:Agilent 5 HC-C18(2)column(250 mmx4.6 mm,5 μm)was adopted.Acetonitrile solution(con-tain 3%tetrahydrofuran)(A)and 0.1%formic acid aqueous solution(B)were used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min-1.The column temperature was 30 ℃ and the injection volume was 20 μL.The detection wavelengths were 210 and 243 nm.Results:The feature profiles developed were effective in identifying the 18 shared peaks.RSD for precision,repeatability and stability(48 h)tests were all less than 3.72%(n=6).The 11 chemical components to be measured were well separated,with good linearity in the mass range examined(all r ≥ 0.999 6).The average recovery rate was 95.4%-105.5%,and the RSD was 1.0%-3.1%.The RSDs of precision,repeatability,and stability(48 h)tests were all less than or equal to 3.0%(n=6).The results of similarity analysis showed that most of the origins of Poriae Cutis were very similar to each other.The results of content determination showed that among the 11 triterpenoid constituents,poricoic acid A accounted for the highest percentage in all batches of Poriae Cutis.In addition,the content of five components,poricoic acid A,dehydrotrametenolic acid,poricoic acid B,dehydroeburicoic acid and trametenolic acid,fluctua-ted relatively more,while the other components fluctuated more gently.No significant geographic variation in sam-ples from different origins.Conclusion:A method for the determination of Poriae Cutis characteristics and multi-component content was established,which laid the foundation for quality control of Poriae Cutis.

Poriae Cutistriterpenoidsspecific chromatogramscontent determinationwavelength conversion

徐凡、袁杰、蒲婧哲、胡冲、张亚中、刘守金

展开 >

安徽中医药大学药学院,合肥 230012

安徽省食品药品检验研究院,合肥 230051

国家药品监督管理局中药质量研究与评价重点实验室,合肥 230051

中药饮片制造新技术安徽省重点实验室,合肥 230012

展开 >

茯苓皮 三萜 特征图谱 含量测定 波长转换

国家重点研发计划

2019YFC1711500

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(2)
  • 15