Rapid Profiling and Characterization of the Multicomponents from the Root and Rhizome of Salvia miltiorrhiza by Ultra-High Performance Liquid Chromatography/Ion Mobility-Quadrupole Time-of-Flight Mass Spectrometry in Combination with Computational Peak Annotation Workflows

Abstract

Herbal components characterization represents a challenging task because of the co-existing of multiple classes of naturally occurring compounds with wide spans of polarity, molecular mass, and the ubiquitous isomerism. The root and rhizome of Salvia miltiorrhiza have been utilized as a reputable traditional Chinese medicine Salviae Miltiorrhizae Radix et Rhizoma (Dan-Shen) in the treatment of cardiovascular disease. Herein, a dimensionenhanced ultra-high performance liquid chromatography/ion mobility/quadrupole time-of-flight mass spectrometry approach in combination with intelligent peak annotation workflows was established aimed to rapidly characterize the multicomponents from S. miltiorrhiza. Due to the sufficient optimization, satisfactory chromatography separation was enabled on an HSS T3 column within 33 min using 0.1% formic acid in water (A) and acetonitrile (B) as the mobile phase, while the data-independent HDMS E in both the negative and positive electrospray ionization modes was utilized for the high-coverage MS 2 data acquisition. Streamlined automatic peak annotation by searching an in-house library (recording 198 known compounds) followed by the subsequent confirming steps (e.g., comparison with the reference compounds, fragmentation pathways analysis, and retention behavior comparison, etc.), allowed us to identify or tentatively characterize a total of 86 components (including 50 terpenoids, 21 phenolic acids, and 15 others) from S. miltiorrhiza. Importantly, three-dimensional structure information, such as the retention time, MS 1 and MS 2 data, and collision cross section (CCS), was provided, which can facilitate the more reliable characterization of herbal components. KEYWORDSUltra-high perform liquid chromatography/ion mobility/quadrupole time-of-flight mass spectrometry; highdefinition MS E ; automatic peak annotation; Salvia miltiorrhiza; phenolic acid; tanshinone

A comprehensive quality evaluation strategy of Shensong Yangxin capsules based on qualitative, fingerprint and quantitative analyses

“…Major fragment ions include m/z 280.1089 [M + H − CH 3 ] + , m/z 277.1235 [M + H − H 2 O] + , m/z 266.0940 [M + H − CHO] + and m/z 249.1261 [M + H − H 2 O − CO] + , which are shown in Figure 13e. The structures of other diterpenoids can be obtained by reference to the law of cracking in the literature (Bharathi et al, 2022; Chen et al, 2022, 2020; Lin et al, 2020).…”

“…Most of the phenolic acids constitute the primary water‐soluble active components extracted from DS. These phenolic acid compounds usually consist of structural units like danshensu and caffeic acid, resulting in the formation of different dimers, trimers, tetramers and salt derivatives (Chen et al, 2022). In this scenario, several phenolic acids display shared fracture behavior, primarily characterized by the depletion of caffeic acid (C 9 H 8 O 4 ,180 Da) and danshensu (C 9 H 10 O 5 , 198 Da), thereby producing characteristic fragment ion peaks.…”

“…The 24 diterpenoids present in SSYXC originate completely from DS, including compounds 85, 86, 90, 96, 97, 100, 101, 103-105, 108, 110, 113, 115, 116, 120, 121, 123-125 and 127-130 in penoids can be obtained by reference to the law of cracking in the literature (Bharathi et al, 2022;Chen et al, 2022Chen et al, , 2020Lin et al, 2020).…”