Formic acid

The LC-MS grade methanol and acetonitrile were purchased from Fisher Scientific (Loughborough, United Kingdom). The mobile phase additive formic acid was from Chem-Lab (Zedelgem, Belgium). Ammonium formate, pentadecanoic acid, pyridine, urease, methoxyamine hydrochloride, N,O-Bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) and alkane standard mixture for GC were from Sigma-Aldrich (United States, Switzerland, Germany). The Milli-Q PLUS system (Millipore, Austria) was used to obtain ultrapure water for sample dilution and urease solution preparation.

Reagents of analytical grade were mainly used, with the exception of mobile phase reagents which were of high-performance liquid chromatography (HPLC) grade. Analytical standards comprised: MPA and NIV from Supelco (Bellefonte, PA, USA); PA from Santa Cruz Biotechnology (Dallas, TX, USA); AFB1, B2, G1, G2, and M1, BEA, CIT, DON, ENNA, and B, FB1 and B2, HT-2 and T-2 toxins, MON, OTA, PAT, TEA, TTX, and ZEA from Sigma-Aldrich (Steinheim, Germany). Ultrapure H₂O was supplied from Millipore System (Paris, France), C18 sorbent from Agilent Technologies (Santa Clara, CA, USA), acetonitrile (ACN) from Carlo Erba (Val de Reuil Cedex, France), anhydrous magnesium sulfate (MgSO₄) and sodium chloride (NaCl) from Honeywell (Seelze, Germany), and formic acid from Chem-Lab (Zedelgem, Belgium). ACQUITY UPLC^® HSS T3 1.8 μm (2.1 × 100 mm i.d.) was purchased from Waters (Milford, MA, USA), and HPLC vials and Syringeless Device Mini UniPrep filters (0.45 μm PVDF, polypropylene) from Whatman (Maidstone, UK).

All solvents used were of LC–MS analytical grade. Acetonitrile was purchased from Carlo Erba (Val De Reuil, France), isopropanol and methanol from Fisher Scientific (Laughborough, UK) and formic acid 98–100% from Chem-Lab (Zedelgem, Belgium). Lauric acid was purchased from Acros Organics (>99%), myristic acid from Sigma Aldrich (>99.5%), myristoleic acid from Sigma Aldrich (>99%), pentadecanoic acid from Sigma Aldrich (>99%), palmitic acid from Fluka (analytical standard), 9-palmitoleic acid from Fluka (analytical standard), margaric acid from Sigma Aldrich (>98%), 10-Z-heptadecenoic acid from Cayman Chemical Company (>98%), stearic acid from Fluka (analytical standard), oleic acid from Fluka (analytical standard), linoleic acid from Sigma Aldrich (>99%), linolenic acid from Sigma Aldrich (>99%), arachidic acid from Cayman Chemical Company (>98%), bihomo-γ-linolenic acid from Cayman Chemical Company (>98%), arachidonic acid from Sigma Aldrich (>99), 5,8,11,14,17-cis-eicosapentanoic acid from Fluka (analytical standard), 7,10,13,16,19-cis-docosapentaenoic acid from Cayman Chemical Company (>98%), 4,7,10,13,16,19-cis-docosahexaenoic acid from Sigma Aldrich (>98%) and lignoceric acid from Cayman Chemical Company (>98%).

All reagents used were characterized by analytical grade. Reagents for the extraction of phenolic compounds and HPLC-DAD analysis were multisolvent and LC-MS quality was chosen for identification purposes using mass spectrometry. Acetonitrile (99.8%) was purchased from Panreac Quimica (Barcelona, Spain); formic acid (99%) and methanol (99.8%) were purchased from ChemLab (Zedelgem, Belgium); diethyl eter (99%) and ethyl acetate (99.9%) were purchased from Fisher chemical (Geel, Belgium); Folin reagent and sodium hydroxide were purchased from LabChem (ACP Chemicals Inc., Zelienople, PA, USA); chloridic acid was purchased from Honeywell Fluka (Buchs, Switzerland); sodium carbonate was purchased from Sigma-Aldrich (Sigma Aldrich, St. Louis, MO, USA); and water was obtained from a Milli-Q^® Direct Water Purification System. Reference standards including those of gallic acid, protocatechuic acid, chlorogenic acid, caffeic acid, catechin, epicatechin, epicatechin gallate, quercetin, quercetin-3-O-glucoside, phlorizin, phloretin, p-coumaric acid, ferulic acid, 4-Caffeyolquinic acid, and kaempferol were acquired from Sigma-Aldrich (Sigma Aldrich, St. Louis, MO, USA).

All reagents used were characterized by analytical grade. Reagents for the extraction of phenolic compounds and HPLC-DAD analysis were multisolvent and LC-MS quality was chosen for identification purposes using mass spectrometry. Acetonitrile (99.8%) was purchased from Panreac Quimica (Barcelona, Spain); formic acid (99%) and methanol (99.8%) were purchased from ChemLab (Zedelgem, Belgium); diethyl eter (99%) and ethyl acetate (99.9%) were purchased from Fisher chemical (Geel, Belgium); Folin reagent and sodium hydroxide were purchased from LabChem (ACP Chemicals Inc., Zelienople, PA, USA); chloridic acid was purchased from Honeywell Fluka (Buchs, Switzerland); sodium carbonate was purchased from Sigma-Aldrich (Sigma Aldrich, St. Louis, MO, USA); and water was obtained from a Milli-Q^® Direct Water Purification System. Reference standards including those of gallic acid, protocatechuic acid, chlorogenic acid, caffeic acid, catechin, epicatechin, epicatechin gallate, quercetin, quercetin-3-O-glucoside, phlorizin, phloretin, p-coumaric acid, ferulic acid, 4-Caffeyolquinic acid, and kaempferol were acquired from Sigma-Aldrich (Sigma Aldrich, St. Louis, MO, USA).

All solvents used were of LC-MS analytical grade. Acetonitrile was purchased from Carlo Erba (Val De Reuil, France), isopropanol and methanol from Fisher Scientific (Loughborough, UK) and formic acid 98% to 100% from Chem-Lab (Zedelgem, Belgium). 10-Hydroxydecanoic acid was purchased from Fluorochem (Derbyshire, UK) and was of the highest available quality. 10-HDA, 3-hydroxydecanoic acid, decanedioic acid and 2-dodecenedioic acid were synthesized in the Laboratory of Organic Chemistry (National and Kapodistrian University of Athens). All physical data were in agreement with literature data and their purity was >97%.

Solutions of analytical standards DON, DON-3G, 3-acetyl-deoxynivalenol (3-AcDON), 15-acetyl-deoxynivalenol (15-AcDON), NIV, FUSX, ZEN, α-ZOL, β -ZOL were purchased from Romer Labs (Tulln, Austria) and ZEN-14S and ZEN-14G were purchased from Aokin (Berlin, Germany). The certified standard of NIV-3G (110 µg/mL) was isolated from wheat according to the procedure described by Yoshinari et al. [45 (link)]. Methanol and water of LC-MS purity were purchased from Witko (Lodz, Poland), formic acid 98–100% (ultrapure) and ammonium formate 97% (extra pure) were purchased from Chem-Lab (Zedelgem, Belgium). Potato-dextrose agar (PDA) was provided by Oxoid (Basingstoke, UK).