Untargeted metabolomics data of orange peel(OP) and fermented orange peel(FOP) extracts by HPLC-Q-TOF-MS

In the subsequent non-targeted metabolomic profiling, FOP or OP powder (1.0 g) underwent ultrasonic extraction in a 25 mL ethanol solution (60%, v/v, HPLC grade) for 30 minutes The extract was then subjected to centrifugation at 6000 rpm for 10 minutes. The supernatant obtained was diluted tenfold with methanol and filtered through a 0.22 μm membrane prior to LC/MS analysis.
Chromatographic analysis was conducted utilizing an ACQUITY HPLC I-Class system in conjunction with a Xevo G3-XS QTOF mass spectrometer (Waters, USA). The chromatographic separation was carried out on a Waters BEH T3 column (1.8 μm, 2.1 mm × 150 mm), which was maintained at a temperature of 40°C. The mobile phase comprised (A) 0.1% formic acid in water and (B) acetonitrile, following a gradient elution program as follows: 0–1 min, 100% to 90% A; 1–3 min, 90% to 60% A; 3–10 min, 60% to 40% A; 10–20 min, 40% to 20% A; 20–27 min, 20% to 90% A; and 27–29 min, 90% A. The flow rate was maintained at 0.3 mL/min, with a detection wavelength set at 350 nm and an injection volume of 10 μL.
In the mass spectrometry analysis, an electrospray ionization (ESI) source was utilized in both positive and negative ionization modes, covering a mass range of 50–1200 Da. MSE data acquisition was conducted under the following conditions: a capillary voltage of 0.5 kV, an ion source temperature of 100°C, a desolvation temperature of 400°C, a desolvation gas flow rate of 800 L/h, a cone voltage of 50 V, and collision energies set at 4 V for low energy and 15–60 V for high energy. Data processing was performed using UNIFI software (version 1.9.2, Waters).
The measured data were compared with the flavonoid library and traditional Chinese medicine library, yielding the following bioactive components, which were then analyzed.