Rapid identification of new minor chemical constituents from Smilacis Glabrae Rhizoma by combined use of UHPLC‐Q‐TOF‐MS, preparative HPLC and UHPLC‐SPE‐NMR‐MS techniques

Abstract

The combination of UHPLC-Q-TOF-MS, preparative HPLC and UHPLC-SPE-NMR-MS techniques is a quick and effective approach for finding new minor constitutes from herbs.

HPLC-PDA-MS/MS Characterization of Bioactive Secondary Metabolites from Turraea fischeri Bark Extract and Its Antioxidant and Hepatoprotective Activities In Vivo

“…In MS 2 , they produced a major ion peak at m / z 613 [M–H–162, loss of a hexose moiety]. In MS 3 of 613, two daughter ions at m / z 503 and 461 were observed; thus, they were identified as bis-dihydroxyphenylpropanoid-substituted catechin hexoside isomers, as reported before [ 13 ] ( Figure 5 a,b and Figure 6 ).…”

“…For instance, peak ( 15 ) at a retention time 33.41 min, exhibited a molecular ion peak [M − H] − ( m / z ) at 451 and two daughter ions at m / z 341 and 299; it was assigned to cinchonain-I, as previously described [ 13 ] ( Figure 3 a). Three peaks ( 8 , 9 , and 10 ) at retention times 25.24, 26.27, and 27.69, respectively, showed [M − H] − ( m / z ) at 613 and three fragment ions at 299, 341, and 451; they were identified as cinchonain-I-hexoside isomers ( Figure 3 b).…”

How close are we to complete annotation of metabolomes?

“…A related project to deeply annotate the metabolome of the NIH model species Daphnia magna (waterflea) is underway in the primary authors’ laboratory, applying multiple extraction methods, LC-MS/MS and MS n methods, GC-Orbitrap MS, and 1D and 2D NMR spectroscopy. Progress has also been reported in the integration of several platforms to enable metabolite identification by UHPLC-SPE-NMR-MS [35]. In addition, approaches such as ion mobility mass spectrometry [36] and ultrahigh resolution mass spectrometry [37] hold considerable promise for contributing to metabolome annotation projects.…”

Recent development in mass spectrometry and its hyphenated techniques for the analysis of medicinal plants

“…For HPLC‐SPE‐NMR‐MS, the chromatographic flow of the sample is first separated in HPLC, and split into two discrete streams; the major proportion of the chromatographic flow is trapped by a SPE device for enrichment and subsequent online or offline NMR analysis, and the remainder is directly detected by MS (Figure ) . The HPLC‐SPE‐NMR‐MS system features the efficient separation and a superb information depth obtained by the concurrent availability of NMR and MS data.…”

“…Among these detection methods, MS is not only characterised by its high sensitivity, excellent resolution, and wide detection dynamic range, but also can be coupled with chromatography for online structural identification of each individual peak . Furthermore, liquid chromatography mass spectrometry (LC–MS) can be interfaced with nuclear magnetic resonance (LC‐NMR‐MS) for more confirmative structure analysis . Thus, MS and its hyphenated techniques have become the major platform for chemical profiling, metabolomics and quality control of medicinal plants in recent years .…”