title: Alkaloid profiling of the Chinese herbal medicine Fuzi by combination of matrix-assisted laser desorption ionization mass spectrometry with liquid chromatography-mass spectrometry.
abstract: A matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) method was developed for the high throughput and robust qualitative profiling of alkaloids in Fuzi--the processed lateral roots of the Chinese herbal medicine Aconitum carmichaeli Debx (A. carmichaeli). After optimization, powdered roots--without any further sample preparation--could be used to screen for the presence of Aconitum alkaloids. Furthermore, the semi-quantitative potential of MALDI-MS was confirmed using liquid chromatography-mass spectrometry (LC-MS) as reference. In total over sixty alkaloids were detected by LC-MS and fifteen of them were tentatively identified. Both MALDI-MS and LC-MS analysis revealed significant variation in alkaloid content in different (commercial) samples. LC-MS analysis of three toxic alkaloids in 14 batches of Fuzi resulted in a variation of their concentrations expressed as RSDs of 138%, 99% and 221% for aconitine, hypaconitine and mesaconitine, respectively. The variation in concentrations (expressed as RSD) of about the ninety constituents detected were classified as follows: 13 constituents showed an RSD of 77-100%, 46 with an RSD of 100-150%, 21 with an RSD of 150-200% and 9 constituents with an RSD in concentration of 200-235%. These results demonstrate a strong difference in chemical composition of the various Fuzi and illustrate the necessity of adequate QA/QC procedures for both safety and efficiency of herbal medicine. The described analytical procedures for alkaloid profiling could play a role in these procedures.
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 116023 Dalian, China.
authors.forename: Jiangshan
authors.initials: J
authors.lastname: Wang
authors.forename: Rob
authors.initials: R
authors.lastname: van der Heijden
authors.forename: Gerwin
authors.initials: G
authors.lastname: Spijksma
authors.forename: Theo
authors.initials: T
authors.lastname: Reijmers
authors.forename: Mei
authors.initials: M
authors.lastname: Wang
authors.forename: Guowang
authors.initials: G
authors.lastname: Xu
authors.forename: Thomas
authors.initials: T
authors.lastname: Hankemeier
authors.forename: Jan
authors.initials: J
authors.lastname: van der Greef
mesh_terms: D000157:Aconitine / Q000031:analogs & derivatives / Q000032:analysis; D031841:Aconitum / Q000737:chemistry*; D000470:Alkaloids / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D004365:Drugs, Chinese Herbal / Q000737:chemistry* / Q000592:standards; D016014:Linear Models; D013058:Mass Spectrometry / Q000379:methods*; D018517:Plant Roots / Q000737:chemistry; D011786:Quality Control; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D000470:Alkaloids; D004365:Drugs, Chinese Herbal; D000157:Aconitine