Rapid Screening and Identification of Diterpenoids in Tinospora sinensis Based on High-Performance Liquid Chromatography Coupled with Linear Ion Trap-Orbitrap Mass Spectrometry

Abstract

Diterpenoids are considered the major active compounds in Tinospora sinensis in virtue of their special structures and activities. Herein, an analytical method was developed for rapid screening and identification of diterpenoids in T. sinensis using high-performmance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry (HPLC-LTQ-Orbitrap) in negative ion mode. Two diterpenoid reference standards were first analyzed to obtain their characteristic ESI-MS/MS fragmentation patterns. Then, based on the extracted ion chromatogram (EIC) data-mining method and characteristic fragmentation pathways analysis, diterpenoids in T. sinensis were rapidly screened and identified. After that, an important parameter, Clog P, was adopted to discriminate between the isomers of diterpenoids. As a result, 63 diterpenoids were characterized from the extract of T. sinensis, including 10 diterpenoids and 53 diterpenoid glycosides. Among them, 15 compounds were tentatively identified as new compounds. Finally, target isolation of one diterpenoid glycoside named tinosineside A was performed based on the obtained results, which further confirmed the deduced fragmentation patterns and identified diterpenoid profile in T. sinensis. The results demonstrated that the established method could be a rapid, effective analytical tool for screening and characterization of diterpenoids in the complex systems of natural medicines.

Molecular level comparison of water extractives of maple and oak with negative and positive ion ESI FT‐ICR mass spectrometry

“…It fits the molecular formulas for deaminoneuraminic acid‐α‐2,6‐lactoside‐β‐OCH 3 and deaminoneuraminic acid‐α‐2,3‐lactoside‐β‐OCH 3. The fourth peak with the formula of C 28 H 37 O 13 could be a tinosposinenside, as detected in the stems of Tinospora sinensis plants . The fifth peak at m/z 551.2134 still possessed a relatively high magnitude (1.4%), but no published information on its identity (C 21 H 37 O 12 ) was available.…”

Analgesic, Anti-Inflammatory, Cytotoxic Activity Screening and UPLC-PDA-ESI-MS Metabolites Determination of Bioactive Fractions of Kleinia pendula

“…Significantly, the hexane fraction showed the most potent cytotoxic effect against all the cancer cell lines tested. The UPLC-PDA-ESI-MS metabolite screening of bioactive hexane fraction revealed the presence of major metabolites including tormentic acid [34], 5-hydroxyadvisiosidec [36], citrostadienyl [37], dehydrated derivative of tinosposinenside B [30] and tinocrisposide [30]. The observed cytotoxic activity could be attributed to the presence of fatty acids and triterpenoid (tormentic acid [47]) in the hexane fraction.…”

Stepwise Diagnostic Product Ions Filtering Strategy for Rapid Discovery of Diterpenoids in Scutellaria barbata Based on UHPLC-Q-Exactive-Orbitrap-MS

“…With the advantage of sensitively acquiring more data, the subsequent disadvantage of this technology is that a large amount of MS data needs a tediously long time for data analysis. In order to achieve the purpose of saving time and improving speed, great efforts have been made to develop more effective MS data post-processing methods such as mass defect filtering (MDF) [ 21 , 22 , 23 , 24 ], neutral loss filtering (NLF) [ 25 , 26 ], extraction ion chromatography (EIC) [ 16 , 27 , 28 ], and so on. These data post-processing techniques simplify the characterization process [ 21 , 22 , 23 , 24 , 25 , 26 , 27 , 28 ], but the exclusion of false positive results and structure confirmation still depends on diagnostic product ions (DPIs) produced in the MS fragmentation.…”