Rapid Separation, Identification and Analysis of Astragalus membranaceus Fisch Using Liquid Chromatography-Tandem Mass Spectrometry
Rapid Separation, Identification and Analysis of Astragalus membranaceus Fisch Using Liquid Chromatography-Tandem Mass Spectrometry
复制标题
DOI：
10.1093/chromsci/bmt016
复制
发表时间：
2014-03-01
影响因子：
1.3
通讯作者：
Zhang, Yan-yan
中科院分区：
文献类型：
--
作者：
Du, Hong-wei;Zhao, Xin-lei;Zhang, Yan-yan
建立了一种快速、灵敏、高选择性的液相色谱-串联质谱（HPLC-MS-MS）联用技术，用于黄芪中化学成分的快速分离和结构鉴定。使用快速HPLC系统与ACQUITY HPLC BEH C18柱，总分析时间为这个复杂的草药是小于30分钟。该方法使用了1.7 μ m颗粒填料，这使得更高的分析速度，峰值容量，更大的分辨率和灵敏度增加的柱。在MS中使用各种碎裂器电压水平时，分子离子和特征碎片离子的准确质量测量（误差小于5 ppm）代表了这些化合物的可靠鉴别标准。根据保留时间、质量裂解行为、MS-MS碎片离子、文献报告和内部分子式数据库的建立，对AR的组分进行了鉴别或初步表征。利用该方法，根据MS数据和与现有数据库的比较，共初步鉴定了22个化合物。总之，快速高效液相色谱-质谱联用技术是一种非常有用和有效的技术，用于分离和鉴定复杂基质中的草药成分。
A rapid, sensitive and selective liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) method has been developed for the rapid separation and structural identification of constituents in Astragali Radix (AR) The analysis was conducted on an ACQUITY HPLC chromatographic instrument and a mass spectrometer using positive electrospray ionization. Using a fast HPLC system with an ACQUITY HPLC BEH C18 column, the total analysis time for this complex herb was less than 30 min. The method used a column with 1.7 mu m particle packing, which allowed a higher speed of analysis, peak capacity, greater resolution and increased sensitivity. With various fragmentor voltage levels in MS, accurate mass measurements (less than 5 ppm error) for molecular ions and characteristic fragment ions represented reliable identification criteria for these compounds. The constituents of AR were identified or tentatively characterized based on their retention times, mass fragmentation behavior, MS-MS fragment ions, literature reports and the establishment of an in-house molecular formula database. With this method, a total of 22 compounds of AR were tentatively identified based on MS data and comparison with available databases. In conclusion, fast HPLC with MS is a highly useful and efficient technique to separate and identify constituents in complex matrices of herbal medicines.