摘要
目的采用UHPLC-Q-Exactive Orbitrap HRMS法对覆盆子Rubus chingii不同部位(小核果和花托)化学成分进行分析鉴定,并建立快速测定覆盆子中9种成分含量的方法。方法采用Acquity UPLC HSS T_(3)(100 mm×2.1 mm,1.8μm)色谱柱,以0.1%甲酸水与乙腈为流动相,梯度洗脱;覆盆子化学成分鉴定时采用正负离子Full MS/dd-MS^(2)模式,通过化合物的一级、二级质谱信息,结合对照品比对确认,进行覆盆子不同部位主要化学成分的快速、精准识别。采用ACQUITY BEH C_(18)(50 mm×2.1 mm,1.7μm)色谱柱在负离子Full MS/SIM模式,建立快速测定覆盆子不同部位中9种成分(没食子酸、芦丁、鞣花酸、金丝桃苷、山柰酚-3-O-芸香糖苷、紫云英苷、椴树苷、槲皮素和山柰酚)含量的UHPLC-Q-Exactive OrbitrapHRMS方法,并测定其含量。结果从覆盆子小核果和花托中共鉴定122种化学成分,包括黄酮类66种、有机酸类28种、萜类24种、其他类4种。成功建立一种6 min完成覆盆子中9种成分含量测定的方法,各成分在其线性范围内线性关系良好;精密度、重复性及稳定性良好(RSD≤6.30%);加样回收率在99.45%~105.30%(RSD≤4.43%),并发现小核果中芦丁的含量显著高于花托;而花托中的鞣花酸、山柰酚-3-O-芸香糖苷和椴树苷的含量显著高于小核果。结论覆盆子小核果和花托部位的化学成分存在差异性,运用UHPLC-Q-Exactive Orbitrap HRMS建立的定量方法分析时间短、灵敏度高、准确性好,方法学考察结果均符合含量测定的要求,可用于覆盆子中9种成分的快速测定。
Objective UHPLC-Q-Exactive Orbitrap HRMS was used to analyze and identify the chemical components in different parts(drupelets and receptacles)of Rubus chingii,and a rapid method for the determination of nine components in drupelets and receptacles of R.chingii was established,and to provide the basis for the rational application of different parts of R.chingii and its quality evaluation.Methods Using Acquity UPLC HSS T_(3)(100 mm×2.1 mm,1.8μm)column with 0.1% formic acid water and acetonitrile as mobile phase,and gradient elution was performed.The identification of chemical components in R.chingii adopted the positive and negative ion Full MS/dd-MS^(2) mode,combined with the primary and secondary mass spectrometry information of the compound,from the comparison and confirmation of reference substances,the main chemical components of R.chingii can be identified quickly and accurately.The UHPLC-Q-Exactive Orbitrap HRMS method for rapid determination of nine components in R.chingii was established by using Acquity BEHC_(18)(50 mm×2.1 mm,1.7μm)column in negative ion Full MS-SIM mode,and the contents of 10 batches of R.chingii were determined.Results A total of 122 chemical components in drupelets and receptacle of R.chingii were identified,including 66 flavonoids,28 organic acids,24 terpenoids and 4 other chemical components.Established a method successfully for the determination of nine components of R.chingii in 6 min,and the linear relationship of each component was good in its linear range.The precision,repeatability and stability were good(RSD≤6.30%);The recoveries were 99.45%-105.30%(RSD≤4.43%).Comparing the average content of nine components in 10 batches of drupelet and receptacle samples,the content of rutin in drupelets is higher than in receptacle,while the contents of ellagic acid,kaempferol 3-rutinoside and tiliroside are higher in receptacles than in drupelets of R.chingii.Conclusion The chemical compositions of different parts(drupelets and receptacles)of R.chingii were different.UHPLC-Q-Exact
作者
沈瑶
黄思红
刘依茹
李靖蕾
陈昌伦
刘考铧
刘伟
秦路平
李荣胜
吴建军
SHEN Yao;HUANG Si-hong;LIU Yi-ru;LI Jing-lei;CHEN Chang-lun;LIU Kao-hua;LIU Wei;QIN Lu-ping;LI Rong-sheng;WU Jian-jun(School of Pharmaceutical Sciences,Zhejiang Chinese Medical University,Hangzhou 310053,China;Department of Pediatric,Baoshan Branch,Shuguang Hospital Affiliated to Shanghai University of Traditional Chinese Medicine,Shanghai 201900,China;Institute of Liver Diseases,Key Laboratory of Liver and Kidney Diseases,Ministry of Education,Shanghai Key Laboratory of Traditional Chinese Clinical Medicine,Shuguang Hospital Affiliated to Shanghai University of Traditional Chinese Medicine(TCM),Shanghai 201203,China)
出处
《中草药》
CAS
CSCD
北大核心
2023年第15期4789-4803,共15页
Chinese Traditional and Herbal Drugs
基金
国家自然科学基金项目(81803794)
浙江中医药大学“5151远志人才工程”(112123A12201/001/004/019)。
