Acetic acid

The N-hexane, ethyl acetate, methanol, ethanol, Folin–Ciocalteu reagent, gallic acid, Sodium carbonate, potassium hydroxide, diethyl ether, phenolphthalein, starch indicator were purchased from Sigma-Aldrich (Steinheim, Germany). Wijs solution (0.1 mol∙L⁻¹ iodine monochloride, acetic acid) was purchased from (Fluka (Steinheim, Germany)), chloroform, acetic acid by (lachner), potassium iodide, sodium thiosulfate by (CHEMPUR (Poland)). The methylene chloride, sodium chloride, sodium sulfate were provided by (Acros Organics (Great Britain)). All of the chemicals used for the analyses were of analytical grade, and all of the test solutions were freshly prepared prior to use.

We used collagen type I rat tail (3.52 mg/mL solution, BD Biosciences), chitosan (low molecular weight, Sigma-Aldrich), genipin (Challenge Bioproducts Co., 98%), acetic acid (Chempur), ethanol 96% (POOH), iron(III) chloride hexahydrate and iron(II) chloride tetrahydrate (Sigma-Aldrich), and ammonia (25% solution, puriss. p.a) (Sigma)

Buffer solutions (polar solvents for HPLC experiments) were prepared by dissolving HPLC-grade ammonium acetate (VWR International, Leuven, Belgium) in ultrapure water obtained from a Milli-Q water purification system (Merck Millipore, Darmstadt, Germany). To adjust the buffer solutions’ pH, two concentrated solutions were used: ammonia (Avantor Performance Materials Poland S.A., Gliwice, Poland) and acetic acid (Chempur, Piekary Śląskie, Poland). HPLC-grade acetonitrile (Chempur, Piekary Śląskie, Poland) and isopropanol (VWR International, Leuven, Belgium) were used as non-polar solvents for HPLC experiments.

1,1-Diphenyl-2-picrylhydrazyl radical (DPPH); 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (Trolox); 2,4,6-tri(2-pyridyl)-s-triazine (TPTZ), dimethyl sulfoxide (DMSO), FeCl₃, acetonitrile, formic acid, sweroside (S), and secologanin (SLo) were acquired from Sigma-Aldrich (Steinheim, Germany). Acetic acid was obtained from Chempur (Piekary Śląskie, Poland). acetonitrile for LC–MS was purchased from POCh (Gliwice, Poland). Cyanidin 3-O-glucoside (Cy 3-glc) and p-coumaric acid (p-CuA), caffeic acid (CA), ferulic acid (FA), quercetin 3-O-glucoside, luteolin 7-O-glucoside (Lglc), luteolin 7-O-rutinoside, diosmin, hesperidin, naringin, rutin, (+)-catechin, (−)-epicatechin, procyanidin B1, loganic acid (LA), and loganin (Lo) were purchased from Extrasynthese (Lyon Nord, France). 5-O-caffeoylquinic acid (5-CQA, chlorogenic acid), 3-O-caffeoylquinic acid (3-CQA, neochlorogenic acid), and 4-O-caffeoylquinic acid (4-CQA, cryptochlorogenic acid) were purchased from TRANS MIT GmbH (Giessen, Germany). All reagents were of analytical grade.

Acetic acid (99.5%), aluminum chloride hexahydrate, copper(II) chloride dihydrate, disodium hydrogen phosphate dihydrate, 96% ethanol, 36% hydrochloric acid, iron(III) chloride hexahydrate, methanol, phosphoric acid, potassium persulfate, potassium dihydrogen phosphate, potassium hexacyanoferrate(III), sodium acetate anhydrous, sodium carbonate anhydrous, sodium hydroxide, sodium nitrite, and trichloroAcetic acid were purchased from Chempur, Poland. Neocuproine was delivered by J&K Scientific, Germany. Folin–Ciocalteu reagent, acetonitrile, iron(II) sulfate heptahydrate, gallic acid were supplied by Merck, Germany, whereas rutin trihydrate by Roth, Germany. ABTS (2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid), DPPH (2,2-diphenyl-1-picrylhydrazyl), TPTZ (2,4,6-tris(2-pyridyl)-s-triazine), Trolox (6-hydroxy-2,5,7,8-tetramethylchromane-2-carboxylic acid), caffeine were purchased from Sigma-Aldrich, USA. All the chemicals were of analytical grade.

Cellulose‐producing strains (K. xylinus E26 (from the in‐house collection), K. xylinus BCRC 12334 (kind courtesy of Prof. Jyh Ming Wu, Department of Chemical and Materials Engineering, Chinese Culture University, Taipei, Taiwan), and K. hansenii ATCC 53582 American Type Culture Collection) were cultured in 10‐ml test tubes filled with 5‐ml of media at 30°C under static conditions for 3 days. One liter culture medium (Hestrin‐Schramm, HS; Hestrin & Schramm, 1954) contained 20.0 g glucose (POCh, Poland), 5.0 g yeast extract (BTL, Poland), 5.0 g bacterial peptone (BTL, Poland), 2.7 g sodium phosphate dibasic (Chempur, Poland), 1.15 g citric acid (Chempur, Poland), and 0.5 g magnesium sulfate (Chempur, Poland). The initial pH of the medium was adjusted to 5.7 with 80% acetic acid (Chempur, Poland). 1% cellulase (from Trichodrma reesei ATCC 26921, Sigma‐Aldrich) was added to the culture, and the released cells were harvested for genomic DNA purification.

Acetic acid, ethanol 96%, methanol, and sucrose were from Chempur (Piekary Śląskie, Poland). HPLC-grade methanol and acetonitrile were purchased in Merck (Darmstadt, Germany).
Plant culture media components, plant growth regulators BA (6-benzyladenine) and NAA (1-naphthaleneAcetic acid) and agar were purchased in Duchefa Biochemie (Haarlem, Netherlands). Cultures were grown in the plant tissue-dedicated glass containers (V8630, Sigma-Aldrich, Saint Louis, MI, USA).
Commercially available standards: chlorogenic acid, cryptochlorogenic acid, and neochlorogenic acid, hyperoside (quercetin 3-galactoside), isoquercitrin (quercetin 3-glucoside), isorhamnetin, kaempferol, guaijaverin (quercetin 3-arabinoside), quercetin, rutoside (quercetin 3-rutinoside), and trifolin (kaempferol-3-galactoside) of HPLC grade (≥95.0%) purity were acquired in Sigma-Aldrich Saint Louis, MI, USA. Ammonium acetate, CuCl₂⋅2H₂O, DPPH, FeCl₃⋅6H₂O, Folin-Ciocalteu reagent, hydrochloric acid (HCl), Na₂CO₃, 2,9-dimethyl-1,10-phenanthroline (neocuprine), 2,4,6-tris(2-pyridyl)-s-triazine (TPTZ), and (±)-6-hydroxy-2,5,7,8-tetramethylchromane-2-carboxylic acid (trolox) were also provided by Sigma-Aldrich. Deionised water (>15 MΩ) was produced in house (PureLab OptionR, Elga, High Wycombe, UK).