The Q-Orbitrap mass spectrometer is an analytical instrument designed for high-resolution, accurate mass measurements of various molecular species. It combines a quadrupole mass analyzer with an Orbitrap mass analyzer to provide precise mass detection and identification capabilities.
The analyses were carried out with an AFADESI23-MSI platform in tandem with a Q-Orbitrap mass spectrometer (Thermo Fisher, United States). In positive ion scanning mode, the spray solvent was composed of acetonitrile: water = 80: 20 (V/V, containing 0.1% formic acid); acetonitrile: water = 80: 20 (V/V) was used for the negative mode. The solvent flow rate was 5 μL/min. Mobile platform parameters and mass spectrum scanning parameters were as follows: Mobile platform parameters: Spectrum scanning parameters:
Liu G.X., Li Z.L., Lin S.Y., Wang Q., Luo Z.Y., Wu K., Zhou Y.L, & Ning Y.P. (2023). Mapping metabolite change in the mouse brain after esketamine injection by ambient mass spectrometry imaging and metabolomics. Frontiers in Psychiatry, 14, 1109344.
Qualitative and Quantitative analysis of DON and degradation products were performed by UHPLC/APCI Q-Orbitrap system consisted of an Ultimate 3000 LC pump and an Ultimate open autosampler coupled with a Q-Orbitrap mass spectrometer (Thermo Fisher Scientific, Bremen, Germany). Mobile phase A of UHPLC was 0.1% formic acid in water, and mobile phase B was acetonitrile. The UHPLC column utilized was a Syncronis C18 100 mm × 2.1 mm, 1.9 μm column (Thermo Fisher Scientific, Bremen, Germany). Gradient profile and flow rates were shown in Table 5. Column oven temperature was set at 30 °C, and autosampler temperature was set at 8 °C. Injection volume was 5 μL, and total run time was 25 min.
Li M., Guan E, & Bian K. (2019). Structure Elucidation and Toxicity Analysis of the Degradation Products of Deoxynivalenol by Gaseous Ozone. Toxins, 11(8), 474.
For SFE, we used an SFT-100 supercritical fluid extractor (Supercritical Fluid Technologies, USA). We also used a LG-02 high speed traditional Chinese medicine pulverizer (Ruian Baixin pharmaceutical equipment factory), Q-Orbitrap mass spectrometer (Thermofisher Scientific, USA), and an Accucore aQ UHPLC column (150 mm × 2.1 mm × 2.6 μm). Key reagents are as follows: oxymatrine, sophocarpine, sophoridine and matrine standard (Tianjin Alta Technology Co., Ltd., batch number 16837-52-8, 6483-15-4, 6882-68-4, 519-02-8) (Fig. 1), mebendazole reference (Tianjin Alta Technology Co., Ltd., batch number 31431-39-7), methyl alcohol as chromatographic purity, CO2 (purity 99.9%, Xining Xingwei Gas Industry Co., Ltd.), isoflurane (Shenzhen Reward Life Technology Co., Ltd.). Sophora moorcroftiana seeds were purchased from Linzhi, Tibet, and identified as the dried seeds of Sophora moorcroftiana by Associate Professor Yang Shibin of Medical College of Qinghai University.
Structural formula of (A) Matrine, (B) Oxymatrine, (C) Sophocarpine, (D) Sophoridine.
Hu C., Gan X., Jia Q., Gao P., Du T, & Zhang F. (2022). Optimization of supercritical-CO2 extraction and pharmacokinetics in SD rats of alkaloids form Sophora moorcroftiana seed. Scientific Reports, 12, 3301.
The MS spectrometry was performed on a Q-Orbitrap mass spectrometer with high resolution (Thermo Scientific, San Jose, United States) using a heat electrospray ionization (HESI) ion source, the main parameters were set as follows: capillary temperature of 320°C, Aux gas flow rate of 10 Arb, spray voltage of 3.5 kV (ESI+)/2.8 kV (ESI–), sheath gas flow rate of 40 Arb (+)/38 Arb (−), the full scan data acquired ranges from 80-1200 m/z with a resolution of 70,000 and a resolution of 17,500 resolution in MS2 mode, samples were analyzed at 20, 30, 40 NCE (normalized collisional energy).
Zhou P., Zhou L., Shi Y., Li Z., Liu L., Zuo L., Zhang J., Liang S., Kang J., Du S., Yang J., Sun Z, & Zhang X. (2021). Neuroprotective Effects of Danshen Chuanxiongqin Injection Against Ischemic Stroke: Metabolomic Insights by UHPLC-Q-Orbitrap HRMS Analysis. Frontiers in Molecular Biosciences, 8, 630291.
The standard reagents of secondary metabolites bassianin (purity ≥ 95%), bassianolide (≥ 95%), beauvericin (≥ 95%), beauveriolide 1 (≥ 95%), enniatins A, A1, and B (≥ 95-99%), and tenellin (≥ 95%) used in this study were purchased from Cayman Chemical (Ann Arbor, MI, USA). Absolute EtOH (HPLC grade, ≥ 99.9%) and MeOH (HPLC grade, ≥ 99.8%) were purchased from J.T. Baker (USA). Deionized water (D.W., ≥18.2 MΩ•cm) was prepared using an ultrapure water system (Arium Pro, Sartorius, Germany). A UPLC system (Thermo Fisher Scientific, Waltham, MA, USA) was equipped with a Q-Orbitrap mass spectrometer (Thermo Fisher Scientific). These instruments were controlled using Xcalibur 4.5 software (Thermo Fisher Scientific).
Kim J.C., Hwang I.M., Kim H.M., Kim S., Shin T.S., Woo S.D, & Park H.W. (2024). Rapid analysis of insecticidal metabolites from the entomopathogenic fungus Beauveria bassiana 331R using UPLC-Q-Orbitrap MS. Mycotoxin research, 40(1).
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