HPLC

HPLC analysis was performed using HPLC equipped with a C18 250 mm × 4.6 mm, 5 μm column . The analysis was maintained at a column temperature of 30℃with an injection volume of 10 μL at a flow rate of 1.0 mL/min. The mobile phase A was methanol and mobile phase B was ultrapure water containing 0.1% (m/v) formic acid. The gradient elution was performed as follows: 0–5 min, B 95–90%, 5–30 min, B 90–80%, 30–45 min, B 80–76%, 45–60 min, B 76–61%, 60–70 min, B 61–57%, 70–80 min, B 57–53%, 80–85 min, B 53–95%, 85–5 min, B 95%. The separated phenolic components were monitored at a wavelength of 280 nm.

来源文献：Zhang X, Li Y, Li Y, Zhao J, Cheng Y, Wang Y, Guan J. Changes of Bioactive Components and Antioxidant Capacity of Pear Ferment in Simulated Gastrointestinal Digestion In Vitro. Foods. 2023 Mar 13;12(6):1211. doi: 10.3390/foods12061211. PMID: 36981138; PMCID: PMC10048753.

UPLCESI-Q-TRAP-MS/MS

C18 column (2.1 mm × 100 mm, 1.8 mm), and the column temperature was maintained at 40℃. The mobile phase consisted of 0.1% formic acid (A) and acetonitrile with 0.1% formic acid (B). Elution gradient: 0–9.0 min, 5–95% B; 9.0–10.0 min, 95–95% B; 10.0–11.1 min, 95–5% B; 11.1–14.0 min, 5–5%. The flow velocity was set as 0.35 mL per minute; The column temperature oven was set to 40℃; the injection volume was 4 mL. The effluent was alternatively connected to an ESI-Q-TRAP-MS. Analyses were conducted on an 4500 Q TRAP . The MS parameters were as follows: source temperature 550℃; ion spray voltage (IS) 5500 V (positive ion mode)/-4500 V (negative ion mode); ion source gas I (GSI), gas II (GSII), curtain gas (CUR) was set at 50, 60, and 25 psi, respectively; the collision-activated dissociation (CAD) was high. QQQ scans were acquired as MRM

experiments with collision gas (nitrogen) set to medium. DP (declustering potential) and CE (collision energy) for individual MRM transitions were done with further DP and CE optimization. A specific set of MRM transitions were monitored for each period according to the metabolites eluted within this period.

来源文献：Xu N, Du LH, Chen YC, Zhang JH, Zhu QF, Chen R, Peng GP, Wang QM, Yu HZ, Rao LQ. Lonicera japonica Thunb. as a promising antibacterial agent for Bacillus cereus ATCC14579 based on network pharmacology, metabolomics, and in vitro experiments. RSC Adv. 2023 May 22;13(23):15379-15390. doi: 10.1039/d3ra00802a. PMID: 37223411; PMCID: PMC10201548.

HPLC

HPLC conditions: chromatographic column was SB-C18 column (4.6 × 250 mm, 5 μm) and the column temperature was maintained at 30℃. The wavelength of ultraviolet detector were 280 nm and 320 nm, and the gradient elution with a flow rate at 0.8 mL/min was performed by mobile phase A (2% acetic acid in deionized water) and solvent B (methanol; 0–10 min, 5–30%; 10–35 min, 30–50%; 35–40 min, 50–60%; 40–45 min, 60–70%; 45–50 min, 70–5%; 50–55 min, 5%).

来源文献：Xu J, Qi Y, Zhang J, Liu M, Wei X, Fan M. Effect of reduced glutathione on the quality characteristics of apple wine during alcoholic fermentation. Food Chem. 2019 Dec 1;300:125130. doi: 10.1016/j.foodchem.2019.125130. Epub 2019 Jul 4. PMID: 31325746.

ESI-Q-TRAP-MS/MS

UPLC conditions: Analyses were conducted on the system with an C18 column (2.1 mm × 100 mm, 1.8 mm), and the column temperature was maintained at 40℃. The mobile phase consisted of 0.1% formic acid (A) and acetonitrile with 0.1% formic acid (B). Elution gradient: 0–9.0 min, 5–95% B; 9.0–10.0 min, 95–95% B; 10.0–11.1 min, 95–5% B; 11.1–14.0 min, 5–5%. The flow velocity was set as 0.35 mL per minute; The column temperature oven was set to 40℃; the injection volume was 4 mL. The effluent was alternatively connected to an ESI-Q-TRAP-MS.

MS conditions: Analyses were conducted on an 4500 Q TRAP . The MS parameters were as follows: source temperature 550℃; ion spray voltage (IS) 5500 V (positive ion mode)/-4500 V (negative ion mode); ion source gas I (GSI), gas II (GSII), curtain gas (CUR) was set at 50, 60, and 25 psi, respectively; the collision-activated dissociation (CAD) was high. QQQ scans were acquired as MRM experiments with collision gas (nitrogen) set to medium. DP (declustering potential) and CE (collision energy) for individual MRM transitions were done with further DP and CE optimization. A specific set of MRM transitions were monitored for each period according to the metabolites eluted within this period.

来源文献：Xu N, Du LH, Chen YC, Zhang JH, Zhu QF, Chen R, Peng GP, Wang QM, Yu HZ, Rao LQ. Lonicera japonica Thunb. as a promising antibacterial agent for Bacillus cereus ATCC14579 based on network pharmacology, metabolomics, and in vitro experiments. RSC Adv. 2023 May 22;13(23):15379-15390. doi: 10.1039/d3ra00802a. PMID: 37223411; PMCID: PMC10201548.

UHPLC

Chromatographic separation of SPLFA and SPLF was done on an Agilent 1290 UHPLC system coupled to an auto sampler, a diode array detector (DAD) and an ACQUITY UHPLC? HSS T3 column (2.1 ×100 mm, 1.8 μm; Waters, Milford, MA, USA)maintained at 30 ℃. Eluent A was 0.05% formic acid in water and eluent B was 0.05% formic acid in acetonitrile. Elution of the SPLPA compounds was achieved using the following linear gradient elution (in %B): 0 min, 5%; 20 min, 60%; 20.1 min, 5%; 30 min, 5%, and for the SPLF compounds: 0 min, 20%, 25 min, 50%, 25.1 min, 20%, 35 min, 20%. The injection volume was 5 μL, with a flow rate of 0.3 mL/ min. All sample solutions were filtered through a 0.22 μm PTFE filter (Agilent Technologies) before analysis. The detection wavelength was 320 nm for SPLPA and 254 nm for SPLF.

来源文献：[1] Luo D , Mu T , Sun H .Profiling of phenolic acids and flavonoids in sweet potato (Ipomoea batatas L.) leaves and evaluation of their anti-oxidant and hypoglycemic activities[J].Food Bioscience, 2020, 39(44):100801.DOI:10.1016/j.fbio.2020.100801.

HPLC

HPLC analysis employed an Agilent 1260 HPLC instrument and a diode array detector (Agilent, Santa Clara, CA, USA). The chromatographic separation was achieved by a Zobax Stablebond Analytical SB-C18 column (250 × 4.6 mm, 5 μm). The mobile phases, containing a gradient of solvent A (acetic/water, 2:98, v/v) and solvent B (acetic acid/acetonitrile/water, 5:50:45, v/v) were used to elute the column. The solvent gradient was programmed from 90% to 55%A and 10% to 45%B for 50 min, 55% to 0%A and 45% to 100%B for 10 min, and 0% to 90%A and 100% to 10%B for 5 min. The flow velocity was 1.0 mL·min-1 , the column temperature was 30℃, and the injection volume was 20 μL

来源文献：Liang D, Deng H, Deng Q, Lin L, Lv X, Wang J, Wang Z, Xiong B, Zhao X, Xia H. Dynamic Changes of Phenolic Compounds and Their Associated Gene Expression Profiles Occurring during Fruit Development and Ripening of the Donghong Kiwifruit. J Agric Food Chem. 2020 Oct 14;68(41):11421-11433. doi: 10.1021/acs.jafc.0c04438. Epub 2020 Sep 30. PMID: 32936614.

HPLC

The phenolic acid contents were also measured usingHigh Performance Liquid Chromatography.Chromatographic separation was conductedwith an C18 column (4.6 mm × 250 mm,5 mm) and a binary solvent system of (A) methanol (0.1%H3PO4) and (B) water (0.1% H3PO4). The elution wasperformed at a flow rate of 1.0 mL/min and the columntemperature was maintained at 30℃. The contents of phenolicacids [CGA, neochlorogenic acid (NCGA), cryptochlorogenicacid (CCGA), p-coumaryl quinic acid, and caffeoyl shikimicacid] were detected at 320 nm and the contents of anthocyanin(cyanidin-3-O-glucoside chloride and cyanidin 3-O-rutinosidechloride) were quantified at 525 nm.

来源文献：Su Z, Jia H, Sun M, Cai Z, Shen Z, Zhao B, Li J, Ma R, Yu M, Yan J. Integrative analysis of the metabolome and transcriptome reveals the molecular mechanism of chlorogenic acid synthesis in peach fruit. Front Nutr. 2022 Jul 19;9:961626. doi: 10.3389/fnut.2022.961626. PMID: 35928835; PMCID: PMC9344011.

UPLC-QTOT-MS

The C18 (2.1 × 100 mm, 1.7 μm) was kept at 30 ℃. The injection volume was 1 μL, and the elution was completed in 18 min with a flow rate of 0.3 mL/min. Solvents A (water + 0.1% formic acid) and B (acetonitrile) were used in the following gradients: 0–2 min (5–10% B), 2–10 min (10–20% B), 10–15 min (20–40% B), 15–17 min (40–70% B), and 17–18 min (70–100% B). The PDA spectra for phenolic compounds were measured at 320 nm and 350 nm. For MS analysis, anthocyanins were analyzed in the positive ion (PI) mode; other phenolic compounds were analyzed in the negative ion (NI) modes. The MS parameters were as follows: source temperature of 120 ℃, desolvation temperature of 250 ℃(400℃ in the positive ion), cone gas flow 50 L/h, desolvation gas flow 600 L/h (800 L/h in the positive ion), source capillary of 3.0 kV. The MS analysis was performed using mass scanning from m/z 50 to 1,500.

来源文献：[1] Xiang Z , Lin C , Zhu Y ,et al.Phytochemical profiling of antioxidative polyphenols and anthocyanins in the wild plant Campanumoea lancifolia (Roxb.) Merr[J].International Journal of Food Properties, 2021, 24(1):105-114.DOI:10.1080/10942912.2020.1867570.