Screening and identification of glycosides in biological samples using energy-gradient neutral loss scan and liquid chromatography tandem mass spectrometry.
A rapid, selective, and reliable strategy has been developed for the screening and identification of glycosides in biological samples: a crude extract was directly infused to a triple-quadrupole MS/MS, and major glycosides were screened out with high confidence by an energy-gradient neutral loss scan (EGNLS) for the loss of sugar(s); then these glycosides were further identified with LC/MS/MS. The proposed EGNLS method was established and optimized with 16 representative glycosides (including ginsenosides and the glycosides of flavones, anthraquinones, and terpenoids). The EGNLS method has two major advantages over the conventional fixed-energy neutral loss scan: (1) The latter is liable to '"omit" some target compounds due to the usual mismatch between the preset collision energy and interested compounds' optimal collision energy (OCE), while EGNLS solves this problem by scanning over an energy range. (2) The EGNLS simultaneously measures the screened compounds' OCE, which not only are essential parameters for further LC/MS/MS analysis but also carry some structural information, as proved by this study. This strategy has been successfully demonstrated with the analysis of glycosides in Scutellaria viscidula Bge and transformed Panaxhairy roots (the glycoside constitutions of both had not been studied before): without laborious separation processes; comprehensive glycoside information on those two plants was obtained by a rapid and simple procedure. This strategy is valuable for the study of glycosides in complex samples.
Qu
Jun
J
Department of Chemistry, School of Life Science and Technology, Tsinghua University, Beijing, PR China.
Liang
Qionglin
Q
Liang
Quonglin
Q
Luo
Guoan
G
Wang
Yiming
Y
D002851:Chromatography, High Pressure Liquid / Q000379:methods; D020719:Glucuronides / Q000032:analysis; D006027:Glycosides / Q000032:analysis* / Q000737:chemistry*; D013058:Mass Spectrometry / Q000379:methods; D015394:Molecular Structure; D010936:Plant Extracts / Q000737:chemistry*; D018517:Plant Roots / Q000737:chemistry; D010946:Plants, Medicinal / Q000737:chemistry; D012680:Sensitivity and Specificity
D020719:Glucuronides; D006027:Glycosides; D010936:Plant Extracts