Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang 050017, China.
J Chromatogr A. 2010 Jul 2;1217(27):4587-600. doi: 10.1016/j.chroma.2010.04.076. Epub 2010 May 6.
The aim of the present study was to develop a practical method for the characterization of coumarins in Radix Glehniae by liquid chromatography-mass spectrometry (LC-MS). First, 10 coumarin standards (including two pairs of isomers) were studied, and mass spectrometry fragmentation patterns and elution time rules for the coumarins were found. Then, an extract of Radix Glehniae was analyzed by the combination of two scan modes, i.e., multiple ion monitoring-information-dependent acquisition-enhanced product ion mode (MIM-IDA-EPI) and precursor scan information-dependent acquisition-enhanced product ion mode (PREC-IDA-EPI) on a hybrid triple quadrupole-linear ion trap mass spectrometer. A total of 41 coumarins were identified on the basis of their mass spectrometry fragmentation patterns. This is the first time that these two scan modes have been combined to characterize chemical constituents in traditional Chinese medicine. This new method allowed the identification of coumarins in Radix Glehniae in trace amounts. The methodology proposed in this study could be valuable for the structural characterization of coumarins from complex natural and synthetic sources.
本研究旨在通过液相色谱-质谱法(LC-MS)建立一种用于鉴定甘松中香豆素的实用方法。首先,对 10 种香豆素标准品(包括两对异构体)进行了研究,发现了香豆素的质谱裂解模式和洗脱时间规律。然后,在混合三重四极杆-线性离子阱质谱仪上,采用两种扫描模式(多离子监测-信息相关采集增强子离子模式(MIM-IDA-EPI)和前体扫描信息相关采集增强子离子模式(PREC-IDA-EPI))对甘松提取物进行了分析。基于质谱裂解模式,共鉴定出 41 种香豆素。这是首次将这两种扫描模式结合起来用于鉴定中药中的化学成分。该新方法能够鉴定甘松中痕量的香豆素。本研究提出的方法可为复杂天然和合成来源的香豆素的结构鉴定提供有价值的方法。