Individual standards of each VMSs (L3–L5 and D3–D6; purity > 97%) and tetrakis(trimethylsilyloxy)silane (M4Q), used as internal standard, were purchased from Sigma-Aldrich (St. Louis, MO, USA). For SPME, two types of fiber, namely 100 µm polydimethylsiloxane (PDMS) and 65 µm PDMS/Divinylbenzene (DVB), were also obtained from Sigma-Aldrich. A Hei-Standard magnetic stirrer with heating from Heidolph Instruments (Schwabach, Germany) was also used in the SPME extraction. Helium (99.999%) used in the GC-FID system, was supplied by Air Liquide (Maia, Portugal).

Individual stock solutions of each siloxane, including the internal standard M4Q, were prepared in n-hexane at 1 g/L. From those individual stock solutions, a 5 mg/L mix stock solution containing all the target analytes were prepared in acetone. A diluted M4Q individual stock solution, with a final concentration of 5 mg/L, was also prepared in acetone. From those stock solutions, new mix solutions with 50 μg/L and 500 μg/L were prepared in acetone. Eight calibration standards in acetone, with concentrations of each analyte ranging from 0.125 μg/L to 5 μg/L (internal standard concentration of 3 μg/L) were also prepared. All the solutions were stored protected from light and at −22 °C.

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