首页|基于UHPLC-MS/MS法分析补肾利咽汤物质基准的特征图谱暨多指标成分的筛选与含量测定研究

基于UHPLC-MS/MS法分析补肾利咽汤物质基准的特征图谱暨多指标成分的筛选与含量测定研究

扫码查看
目的 采用超高效液相-质谱(UHPLC-MS/MS)法同时测定补肾利咽汤(BSLYT)中化学成分,建立BSLYT物质基准的高效液相色谱指纹图谱及莫诺苷、马钱苷、木蝴蝶苷A、木蝴蝶苷B、黄芩苷、落新妇苷等6种主要成分的含量测定方法,为质量控制提供参考。方法 利用质谱数据,建立指纹图谱。用外标法计算BSLYT样品中主要成分的含量,并结合化学计量学方法分析不同批次样品的差异。结果 质谱共指认出了69种化合物,经过与高效液相色谱比对,共指认出13种化合物。15批BSLYT物质基准特征图谱的相似度在0。90以上,共指认了27个共有峰。聚类分析(CA)将物质基准分为2类,即S1、S2、S5、S8、S9、S13、S15为一类,S3、S4、S6、S7、S10-S12、S16为一类。通过主成分分析(PCA)和正交偏最小二乘法判别分析(OPLS-DA),筛选出影响物质基准分类的化学成分,分别归属于木蝴蝶、山茱萸和土茯苓。多指标成分含量测定6个成分,分别为莫诺苷、马钱苷、木蝴蝶苷A、木蝴蝶苷B、黄芩苷、落新妇苷含量范围分别在0。31%-0。51%、0。12%-0。22%、0。09%-0。19%、0。09%-0。24%、0。07%-0。18%、0。08%-0。29%。结论 本文建立的指纹图谱和多指标含量测定方法准确、稳定,为补肾利咽汤的物质基准及相关制剂的质量控制提供依据。
Study on the Characteristic Spectra and Multi indicator Component Screening and Content Determination of BSLYT Substance Standards Based on UHPLC-MS/MS Method
Objective To determine the chemical constituents in BSLYT by ultra-high performance liquid chromatography-mass spectrometry(UHPLC-MS/MS),and to establish a high-performance liquid chromatographic fingerprint of the material basis of BSLYT and the content determination of its six main constituents,mononoside,loganin,oroxin A,oroxin B,baicalein and astilbin,providing a reference for the quality control.Methods The mass spectrometry data were used to establish the fingerprints.The content of the main components in the BSLYT samples was calculated by using the external method,and the discrepency between different batches of samples were analyzed by combining with chemometric methods.Results A total of 69 compounds were identified by mass spectrometry,and 13 compounds were identified after comparison with high-performance liquid chromatography(HPLC).The similarity of the baseline characterization profiles of the 15 batches of BSLYT substances was above 0.90,and a total of 27 common peaks were identified.Cluster analysis(CA)classified the substance benchmarks into 2 classes,S1,S2,S5,S8,S9,S13,and S15 were clustered into one class,and S3,S4,S6,S7,S10-S12,and S16 were clustered into one class.By combining PCA and OPLS-DA,the chemical components affecting the baseline classification of the substances were screened and attributed to wood butterfly,cornelian cherry and cocos nigra,respectively.The contents of six components were determined by MICS,which ranged from 0.31%-0.51%,0.12%-0.22%,0.09%-0.19%,0.09%-0.24%,0.07%-0.18%,and 0.08%-0.29%for mononoside,loganin,oroxin A,oroxin B,baicalein and astilbin respectively.Conclusion The fingerprint and multi-indicator content determination method established in this paper are accurate and stable,which provide a basis for the quality control of the material benchmark of Kidney and Pharynx Formula and its related preparations.

BSLYTMaterial basisUltra-high performance liquid chromatography-mass spectrometryFingerprintContent determinationChemometric

赵威、马永璠、刘忠义、宋丽敏、刘艳华、张守琳、初洪波

展开 >

长春中医药大学药学院 长春 130117

长春中医药大学第一附属医院 长春 130021

长春中医药大学第一附属医院实验中心 长春 130021

补肾利咽汤 物质基准 超高效液相-质谱 指纹图谱 含量测定 化学计量学

吉林省科技厅科技发展计划重点研发类型项目

20220204056YY

2024

世界科学技术-中医药现代化
中科院科技政策与管理科学研究所,中国高技术产业发展促进会

世界科学技术-中医药现代化

CSTPCD北大核心
影响因子:1.175
ISSN:1674-3849
年,卷(期):2024.26(3)
  • 40