Qualitative and quantitative determination of Atractylodes rhizome using ultra‐performance liquid chromatography coupled with linear ion trap–Orbitrap mass spectrometry with data‐dependent processing

Abstract

A quick and effective workflow based on ultra-performance liquid chromatography coupled with electron spray ionization and LTQ-Orbitrap mass spectrometry (UPLC-LTQ-Orbitrap MS) was established for compositional analysis and screening of the characteristic compounds of three species of Atractylodes rhizome for quality evaluation. This technique was employed to determine the seven main components in Atractylodes rhizome samples. Ultimately, 78 constituents were identified; of these, seven characteristic compounds were selected for species discrimination, comprising atractylodin (63), atractylenolide I (43), atractylenolide II (49), atractylenolide III (53), atractylon (69), methyl-atractylenolide II (54) and (4E,6E,12E)-tetradecadecatriene-8,10-diyne-1,3-diacetate (59). The seven main compounds, including six characteristic compounds, were simultaneously determined in 29 batches of Atractylodes rhizome samples. Thus, the method validation showed acceptable results. Quantitative analysis showed significantly different contents of the seven main components among the three species of Atractylodes rhizome, which indicates possible distinctions in the pharmacological effects. This established method can simultaneously provide qualitative and quantitative results for compositional characterization of Atractylodes rhizomes and for quality control.

UPLC-Q-Exactive Orbitrap MS Analysis for Identification of Lipophilic Components in Citri Sarcodactylis Fructus from Different Origins in China Using Supercritical CO2 Fluid Extraction Method

“…Compound 31 (fragmentation pathway is shown in Figure H) exhibited the [M + H] + ion at m / z 233.1539 in the MS spectrum, and the main fragment ion peaks were at m / z 187.1486, m / z 177.0712, m / z 151.0756, m / z 131.0858, m / z 105.0703, and m / z 91.0549. Therefore, compound 31 was confirmed as atractylenolide II from a previous report . Compound 35 produced a molecular ion peak at m / z 231.1380 for [M + H] + and daughter ions like m / z 213.1274, m / z 185.1325, and m / z 147.0800.…”

Qualitative Analysis of Drug-Containing Plasma and its Application to Quantitative Analysis and Pharmacokinetic Study of Zexie Decoction Using UPLC-MS/MS

“…Parts of representative and potential bio-active compounds in ZX and BZ were chosen to clarify their second-order mass spectrometry graphs and proposed fragmentation pathways, including 16-oxo-alisol A, alisol B, alisol B 23-acetate, alisol C 23-acetate, alisol F, alisol I, atractylenolide I, II and III ( Liu et al, 2010 ; Chao et al, 2016 ; Chen et al, 2016 ; Li et al, 2016 ; Bi et al, 2017 ; Na Yang et al, 2020 ; Kanno et al, 2017 ; Fei et al, 2018 ; Zhang et al, 2018 ; Chang et al, 2021 ). Detailed descriptions were as follows.…”

Identification of lipophilic components in Citri Reticulatae Pericarpium cultivars by supercritical CO2 fluid extraction with ultra‐high‐performance liquid chromatography–Q Exactive Orbitrap tandem mass spectrometry

“…Compound 42, for example, was designated as atractylenolide II based on the related literature [30] with a [M+H] + peak at m/z 233.1537 and fragment peaks at m/z 215.1434 [M+H‐H 2 O] + , 187.1483 [M+H‐H 2 O‐CO] + , and 159.1170 [M+H‐H 2 O‐CO‐C 2 H 4 ] + . Its detailed fragmentation pattern is displayed in Figure 4e.…”