Ennb1

Reagents and chemicals employed are described in detail in a previous work [31 (link)].
Methanol (MeOH) and acetonitrile (ACN), (HPLC grade) and Chloroform (CHCl3) (99% grade) were purchased from Merck (Darmstadt, Germany). Ethyl acetate (EtOAc) (HPLC grade 99.5+%) was supplied by Alfa Aesar (Karlsruhe, Germany). Deionized water (resistivity > 18 MΩ cm⁻¹) was obtained from a Milli-Q SP^® Reagent Water System (Millipore Corporation, Bed-ford, MA, USA). Ammonium formate salt (99%) was obtained from Panreac Quimica S.A.U. (Barcelona, Spain) and sodium chloride (NaCl) was supplied by VWR Chemicals (Leuven, Belgium). Formic acid (reagent grade ≥ 95%) was supplied by Sigma-Aldrich (St. Louis, MO, USA). Enniatin standards (ENNA, ENNA1, ENNB and ENNB1) were purchased from Sigma (St. Louis, MO, USA).

Methanol (MeOH) and acetonitrile (MeCN) of LC-MS grade, and ammonium formate were supplied by VWR International Eurolab S.L. (Barcelona, Spain). Formic acid eluent additive for LC–MS was obtained from Sigma Aldrich (St. Louis, MO, USA). Magnesium sulphate (MgSO₄), sodium chloride (NaCl) and sodium citrate were purchased from Panreac Química (Barcelona, Spain), while disodium hydrogen citrate sesquihydrate was supplied by Merck (Darmstadt, Germany). Ultrapure water was obtained from a Milli-Q Plus system (Millipore Bedford, MA, USA).
Mycotoxin standard solutions (10 mg/L in MeCN) of OTA, STE, F-X, DON, CIT, ZEN, FB1, FB2, T-2 and HT-2 were purchased from Techno Spec (Barcelona, Spain). Individual standards (powder) of ENNA, ENNA1, ENNB, ENNB1 and BEA were obtained from Sigma Aldrich and stock solutions were prepared at 1000 mg/L in MeCN. Multi-mycotoxins intermediate working solutions in MeCN (1 mg/L of OTA and STE; 2 mg/L of CIT; 10 mg/L of FB1, FB2, T-2, HT-2 and ZEN; 100 mg/L of DON, ENNA, ENNA1, ENNB, ENNB1 and BEA and 1000 mg/L of F-X) were prepared by combining suitable aliquots of each individual standard stock solution. These solutions were stored at −20 °C.
Nylon syringe filters (13 mm, 0.22 μm, from VWR) were used for filtration of extracts prior to the injection into the chromatographic system.

ENNA1, ENNB1, and ENNB standards were purchased from Sigma-Aldrich (Steinheim, Germany); DON and AFB1 standards from LGC (Teddington, UK); and BEA and ZEN standards from Dr. Ehrenstorfer (Augsburg, Germany). Individual stock solutions were prepared at 100 μg/mL in dimethylsulfoxide (DMSO), except for BEA, which was prepared at 100 µg/mL in acetonitrile (ACN) and DON at 500 µg/mL in methanol (MeOH). Working standard solutions were prepared by appropriately diluting the stock standard solutions with ACN and stored in amber vials at −20 °C. HPLC-grade ACN and MeOH were purchased from Sigma-Aldrich (Steinheim, Germany). Ammonium formate, 99% purity, and NaCl were purchased from Sigma-Aldrich (Steinheim, Germany). Formic acid and acetic acid were acquired from Honeywell Fluka (Seelze, Germany). Bulk Extrabond^® C18, PSA, and MgSO₄ were obtained from Scharlab (Barcelona, Spain). Ultrahigh-purity water (H₂O) was obtained from a MilliQ water purification system (Millipore, Madrid, Spain).