An integrated strategy of MS-network-based offline 2DLC-QTOF-MS/MS coupled with UHPLC-QTRAP®-MS/MS for the characterization and quantification of the non-polysaccharides in Sijunzi decoction

Abstract

Graphical abstract Sijunzi decoction (SJZD), a classic recipe in traditional Chinese medicine (TCM), has been applied for the clinical treatment of gastrointestinal diseases. While there are reports on pharmaceutical substances of SJZD focusing on its polysaccharides, the composition of non-polysaccharides (NPSs) has not yet been holistically clarified. In the current study, offline two-dimensional liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (2DLC-QTOF-MS/MS) was used for comprehensive NPS chemical profiling of SJZD. In addition, the MS-network of SJZD was proposed, which led to the construction of a larger in-house chemical library and accelerated qualitative processing. Four hundred forty-nine components, among which 6 were potentially novel, and 32 were confirmed by standard substances, were identified or tentatively assigned. Furthermore, based on good method validation, 19 representative components were simultaneously quantified by ultra-high-performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry (UHPLC-QTRAP ® -MS/MS). They were selected for quantification on the account of their bioactive reports on in vivo or in vitro activities, the peak intensity in the mass spectrum, and characteristic structures, which have the potential to be qualitative or quantitative markers of SJZD. The present work furthers understanding of the pharmacological effects and action mechanism of NPSs in SJZD, and provides a useful analytical approach for complex composition research of TCMs. Supplementary Information The online version contains supplementary material available at 10.1007/s00216-021-03302-x.

Multiple approaches to characterize and visualize the chemical composition of Sijunzi Decoction comprehensively

“…These components not only had low contents in SJZD decoction but were also easily lost during the sample preparation process, which increased the difficulty of determination. Therefore, according to the established method, the 18 compounds in SJZD decoction were detected [10], as shown in Figure 6 and Table S10. The content of total saponins in SJZDP was relatively high, such as ginsenoside Re (3.565 ± 0.161 mg/g), ginsenoside Rb1 (3.672 ± 0.224 mg/g), glycyrrhizic acid (3.905 ± 0.235 mg/g), followed by flavonoids, liquiritin apioside (1.024 ± 0.022 mg/g), liquiritin (1.287 ± 0.056 mg/g), and there was a small amount of lactones, atractlenonetin III (0.098 ± 0.032 mg/g).…”

“…The determination of 18 compounds in SZJD decoction was referred to as the method established in the laboratory [10] and was performed based on UPLC coupled with triple‐quadrupole linear ion‐trap MS/MS. Chromatographic separation was performed on a Shimadzu LC‐30A UHPLC system (Kyoto, Japan) consisting of an autosampler (SIL‐30AC) and a binary pump (LC‐30AD).…”

“…A recent study demonstrated that the non-polysaccharides component (NPS) and active polysaccharides in SJZD showed different efficacy on spleen deficiency syndrome [8]. In addition, qualitative and quantitative analyses of NPS were carried out previously [9,10]. Nevertheless, the content of different types of ingredients is still not clarified clearly, it is still important to fully reveal the chemical composition of SJZD.…”

Network Pharmacology and Experimental Verification Revealed the Mechanism of Yiqi Jianpi Recipe on Chronic Obstructive Pulmonary Disease

“…The preparation of YQJPR sample was performed as Dong et al [ 8 ] and improved. Ten herbs were included in YQJPR, which were Huang Qi 30 g, Dang Shen 20 g, Bai Zhu 12 g, Fu Lin 15 g, Zhu Li Ban Xia 12 g, Chen Pi 9 g, Qian Hu 12 g, Dan Pi 12 g, and Gan Cao 3 g. All the above herbs (125 g in total) were mixed with boiling water and boiled twice (1.5 h for the first time, the amount of water was 8 times the quality of the herbs that was 1000 ml; 0.5 h for the second time, the amount of water was 6 times that was 750 ml).…”

Combining multidimensional chromatography-mass spectrometry and feature-based molecular networking methods for the systematic characterization of compounds in the supercritical fluid extract of Tripterygium wilfordii Hook F

“…Conventional one-dimen-sional separation methods have significant methodological limitations in chromatographic separation and peak capacity. 10 Two-dimensional liquid chromatography is an effective method based on integrating different separation mechanisms to improve peak capacity and resolution. 11 Compared with online 2D chromatography, the advantages of offline 2D chromatography systems include their compatibility with solvents and ease of use, which makes them a powerful tool for research into natural products.…”