After the addition of 4 g of NaCl (≥99.5%, Sigma-Aldrich, St. Louis, MO, USA) and stirring bar of 20 mm × 5 mm, the vial was capped with a silicone/polytetrafluoroethylene septum and an aluminum cap (Chromacol Ltd., Herts, UK). The samples were stored at −80 °C until analysis.