摘要
目的:基于超高效液相色谱-线性离子阱-静电场轨道阱高分辨质谱系统(UPLC-LTQ-Orbitrap-MS)分析鉴定中药瓜蒌的化学成分。方法:瓜蒌样品粉碎过筛后采用70%甲醇超声提取,WatersHSST3-C18色谱柱(2.1mm×100mm,1.8μm),流动相0.1%甲酸水溶液-甲醇梯度洗脱,流速0.3mL·min^-1,采用电喷雾离子源(ESI),正、负离子分别进行一级、二级质谱数据采集。为了获得更多的化合物信息,根据色谱峰分离情况、质谱响应强度以及一级质谱解卷积后提取得到的准分子离子数量,优化样品提取条件、色谱及质谱参数。根据精确相对分子质量、离子碎片信息、相关对照品比对,并结合瓜蒌化学成分文献信息,对其中的化学成分进行分析鉴定。结果:从瓜蒌中共分析鉴定了91个化学成分,包括14个氨基酸类化合物,5个单萜类化合物,5个四环三萜类化合物,1个五环三萜类化合物,14个黄酮类化合物,17个有机酸类化合物,3个多糖类化合物,7个核苷类化合物,7个生物碱及含氮化合物,12个挥发性成分,1个植物甾醇,及其他5种化合物。结论:该方法具有高效分离、高灵敏检测优势,可较为全面地对瓜蒌中不同类型化合物进行分析鉴定,为瓜蒌药效物质基础及质量标准研究提供参考。
Objective: To analysis and identify the chemical components in Trichosanthis Fructus by UPLC-LTQ-Orbitrap-MS. Method: Samples of Trichosanthis Fructus were extracted by ultrasonic with 70%methanol after smashing and sifting by 40 mesh sieve. Thermo ScientificTMDionexTMUlti MateTM3000 Rapid Separation LC system performed UPLC separations with Waters HSS T3-C18(2. 1 mm × 100 mm,1. 8 μm)column. The mobile phase was 0. 1% formic acid water(A)-methanol(B) with a gradient elution. The volume flow was 0. 3 mL·min-1. A Thermo ScientificTMLTQ-Orbitrap mass spectrometer equipped with a ESI probe was employed. The samples were respectively scanned in MS1 and MS2 mode of positive and negative ions. According to the chromatographic peak separation,mass signal intensity,and the number of molecular ions in MS1 model,the extraction condition,chromatogram and mass spectrum parameters were optimized. The chemical compounds were identified by the accurate mass measurement of molecular ions and fragment ion and comparation with reference substance. Result: 91 chemical compositions in Trichosanthis Fructus were totally identified,including 14 amino acids,5 monoterpenoids,5 tetracyclic triterpenoids,1 pentacyclic triterpene,14 flavonoids,17 organic acids,3 polysaccharides,7 nucleotides,7 alkaloids and nitrogen compounds,2 volatile components,1 phytosterol,5 other compositions. Conclusion: The established UPLC-LTQ-Orbitrap-MS method can be used to quickly analyze and identify the main chemical constituents of Trichosanthis Fructus. The chemical information concerning the constituents in Trichosanthis Fructus could be helpful to the quality control and further studies of Trichosanthis Fructus.
作者
李欣
唐力英
许静
于现阔
杨洪军
李德凤
张毅
范建伟
苏瑞强
吴宏伟
张琼
LI Xin;TANGLi-ying;XU Jing;YU Xian-kuo;YANG Hong-jun;LI De-feng;ZHANG Yi;FAN Jian-wei;SU Rui-qiang;WU Hong-wei;ZHANG Qiong(School of Pharmacy,Shanxi Medical University,Taiyuan 030001,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Belting 100700,China;State Key Laboratory of Generic Manufacture Technology of Chinese Traditional Medicine,Lunan Pharmaceutical Group Co.Ltd.,Linyi 276006,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2019年第1期201-210,共10页
Chinese Journal of Experimental Traditional Medical Formulae
基金
山东省重大科技创新工程-“中医精方”重大科技创新工程项目(2018CXGC1305)
国家自然科学基金项目(81403210)