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Analysis of bufadienolides in the Chinese drug ChanSu by high‐performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometry
Author(s) -
Ye Min,
Guo Dean
Publication year - 2005
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1989
Subject(s) - chemistry , atmospheric pressure chemical ionization , chromatography , fragmentation (computing) , tandem mass spectrometry , mass spectrometry , bufalin , chemical ionization , high performance liquid chromatography , ionization , ion , organic chemistry , biochemistry , apoptosis , computer science , operating system
Abstract The qualitative analysis of bufadienolides in the Chinese drug ChanSu was performed using high‐performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometry (APCI‐MS/MS). Bufadienolides are the major bioactive constituents of ChanSu, which is used to treat heart failure and cancer in traditional Chinese medicine. The APCI‐MS fragmentation behavior of bufadienolides was studied. For bufadienolides with only hydroxyl substituents, the fragmentation was characterized by successive eliminations of H 2 O and CO molecules, and the profile of MS/MS product ions was correlated with the number of hydroxyl groups. If a C‐16 acetoxyl group was present, the fragmentation of [M+H] + ions was triggered by initial loss of 60 Da (HOAc). The elimination of CO was significant for bufadienolides with a 19‐formyl group, and the 19‐hydroxyl group could be characterized by the loss of 30 Da (HCHO). These fragmentation rules were applied to the identification of bufadienolides in a methanolic extract of ChanSu, which was separated on a C 18 column with gradient elution. A total of 35 bufadienolides were identified, including four new constituents. The method established here facilitated the convenient and rapid quality control of ChanSu crude drug and its pharmaceutical preparations. Copyright © 2005 John Wiley & Sons, Ltd.