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Each sample (10 mg) was accurately weighed and extracted with 1 mL of D2O containing 0.5 mM DSS as an internal standard. The extraction was performed using sonication for 30 min.

After extraction, the suspensions were centrifuged at 14,000×g for 7 min at rt. Subsequently, 600 μL of the supernatant was transferred into 5-mm NMR tubes for analysis.

One-dimensional 1H NMR spectra was acquired at 298 K on a Bruker Avance III HD 500 MHz NMR spectrometer (Bruker BioSpin, Germany) with a Bruker 5 mm BBO probe.