基于指纹图谱与含量测定的地骨皮与焙地骨皮质量评价  

Quality Evaluation of Lycii Cortex and Roasted Lycii Cortex Based on Fingerprint and Content Determination

作　　者：吴沂桓 曾文莉 秦雪梅[2] 石宗鑫 黄程成 代云桃[1,2] WU Yihuan;ZENG Wenli;QIN Xuemei;SHI Zongxin;HUANG Chengcheng;DAI Yuntao(Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Modern Research Center for Traditional Chinese Medicine,Shanxi University,Taiyuan 030006,China;Hubei Meisichuang Pharmaceutical Co.Ltd.,Jingzhou 434000,China)

机构地区：[1]中国中医科学院中药研究所,北京100700 [2]山西大学中医药现代研究中心,太原030006 [3]湖北美思创药业有限公司,湖北荆州434000

出　　处：《中国实验方剂学杂志》2025年第2期165-172,共8页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家重点研发计划项目(2023YFC2308200);中国中医科学院中药研究所重点专项(CI2023E001TS03)。

摘　　要：目的:构建地骨皮的指纹图谱及含量测定方法,为地骨皮及焙地骨皮质量标准制定提供科学依据。方法:采用高效液相色谱法(HPLC),通过Alphasil XD-C_(18) CH色谱柱(4.6 mm×250 mm,5μm),建立地骨皮与焙地骨皮中地骨皮乙素的定量方法。建立10批地骨皮与焙地骨皮的HPLC指纹图谱,并利用超高效液相色谱-四极杆-飞行时间质谱法(UPLC-Q-TOF-MS)基于对照品、文献和质谱信息对标定的共有峰进行指认。以饮片得率、外观性状、地骨皮乙素含量及指纹图谱为质量评价指标,对地骨皮焙制的温度、时间进行考察,筛选最佳炮制工艺,并进行验证。同时,结合化学模式识别,评估地骨皮焙制前后,以及不同产地样品间的化学组成差异。结果:含量测定结果显示,地骨皮和焙地骨皮中地骨皮乙素的质量分数分别为0.35%~5.51%、0.24%~4.15%,焙制后地骨皮乙素转移率为58.6%~78.9%。指纹图谱分析结果显示,该研究建立的方法能有效分离样品中的地骨皮乙素与其他成分色谱峰,并能将对照品地骨皮乙素与其杂质峰顺式咖啡酰丁二胺清晰分离。地骨皮和焙地骨皮的HPLC指纹图谱相似度均>0.95,标定了7个共有峰,并指认了地骨皮乙素、顺式咖啡酰丁二胺、香豆酰酪胺、阿魏酰基丁二胺、丁香酸葡萄糖苷5个共有成分。经工艺优化,确定了110℃焙制20 min为稳定可行的地骨皮焙制工艺。主成分分析和聚类分析显示,生地骨皮与焙地骨皮整体化学组成差异较小,但不同产地地骨皮间质量存在较大差异。结论:该研究建立了地骨皮与焙地骨皮的指纹图谱与有效成分地骨皮乙素的定量方法。通过定性、定量分析,明确了焙制对地骨皮化学组成的影响低于其产地差异。该研究结果为地骨皮及其炮制品的质量评价方法的建立和质量标准的制订提供参考和依据。Objective:To establish fingerprint profiles and a quantitative determination method for Lycii Cortex,providing a scientific basis for the formulation of quality standards for Lycii Cortex and its roasted products.Methods:High performance liquid chromatography(HPLC)was developed for the quantitative method for determining kukoamine B in Lycii Cortex and its roasted products on an Alphasil XD-C_(18) CH column(4.6 mm×250 mm,5μm).HPLC fingerprint profiles were established for 10 batches of Lycii Cortex and its roasted products,and ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS)was used to identify the common peaks based on reference standards,literature and MS information.Quality evaluation indicators included yield of decoction pieces,appearance properties,content of kukoamine B,and fingerprint profiles.The temperature and time of the roasting process were investigated to select the optimal preparation process,which was then verified.Additionally,chemical pattern recognition was combined to assess the differences in the chemical composition of Lycii Cortex before and after roasting,as well as among samples from different origins.Results:Quantitative analysis indicated that the contents of kukoamine B in Lycii Cortex and its roasted products were 0.35%-5.51% and 0.24%-4.15%,respectively.The transfer rate of kukoamine B was 58.6%-78.9% after roasting.The fingerprint profile analysis demonstrated that the method established in this study effectively separated kukoamine B from other components in the samples and distinctly differentiated it from its impurity peak,cis-N-caffeoylputrescine.The HPLC fingerprint profiles of Lycii Cortex and its roasted products showed high similarity(all above 0.95),with 7 common peaks identified and five common components,including kukoamine B,cis-N-caffeoylputrescine,N-coumaroyl tyramine,feruloyltyramine,and glucosyringic acid,confirmed.Process optimization confirmed that baking at 110℃ for 20 min was a stable and feasible method for

关 键 词：地骨皮 焙地骨皮 炮制工艺 地骨皮乙素 质量评价 指纹图谱 高效液相色谱法(HPLC) 超高效液相色谱-四极杆-飞行时间质谱法(UPLC-Q-TOF-MS) 

分 类 号：R277[医药卫生—中医学] R943.1[理学—分析化学] O657[理学—化学]