Supelclean envi florisil

Fipronil, cypermethrin, and tebuconazole standards, surrogate standard delta-hexachlorocyclohexane (δ-HCH), and labeled internal standard phenanthrene-D10 were obtained from Sigma-Aldrich (purity >97%, USA) for use in this study. All employed solvents (n-hexane, acetone, and toluene) were of HPLC grade (J.T. Baker, Netherlands). Glass fiber filters (47 mm, pore size 1.6 µm, Whatman, England), Supelclean ENVI-Florisil (500 mg/3 mL, Sigma-Aldrich, USA) normal-phase cartridges, and activated carbon (Merck, Darmstadt, Germany) were used for solid-phase extraction. The general physicochemical properties of Fipronil, cypermethrin, and tebuconazole are given in Supplemental Table S1.

The analysis was done according to the laboratory protocol and the protocols described by Vaiano et al. (9 (link), 10 (link)). Solid-phase extraction was performed using the Supelclean Envi Florisil and Supelclean LC-18 for reversed-phase extraction (Supelco, Sigma Aldrich, Taufkirchen, Germany). For liquid-liquid extraction we used TOXI Tubes A (Varian, Palo Alto, CA, USA). Drugs were qualitatively analysed with a Shimadzu GC/MS-QP2010 Ultra (Shimadzu, Kyoto, Japan) gas chromatograph with mass spectrometer using the full-scan mode (m/z range 40–600). The chromatographic column was InterCap 5MS/NP (5 % phenyl-95 % methyl polysiloxane, length 30 m, diameter 0.25 mm, film thickness 0.25 μm). The initial column temperature of 90 °C was held for 3 min, then increased to 270 °C at 15°C/min and held there for 5 min, and then increased to 320 °C at 15 °C/min and held there for 27 min. The total run time was 50.33 min. Ultra-pure grade helium was used as a carrier gas at the flow rate of about 1.5 mL/ min.
The obtained data were compared with the Wiley mass spectra library of designer drugs (DD2015), the SWGDRUG free database, and our own in-house library containing about 1000 compounds and metabolites (11 , 12 ). Each sample was analysed twice.