Hp 5972

The solvents were distilled, dried and stored according to standard procedures.²⁰ Unless otherwise stated, reagents were obtained from commercial sources and were used as received. The imidazolium salts were synthesized according to our previously reported method.^{14 (link)1}H, ¹³C NMR, and 2D-HSQC spectra were recorded with a Bruker Advance 300 spectrometer. Chemical shifts (δ) are reported in ppm with the residual solvent resonance signal: δ H/C 7.27 : 77.2 for CDCl₃; and δ H 4.79 for D₂O. Melting points were determined on a Reichert–Kofler hot-stage microscope and were uncorrected. Microanalytical data were obtained using an Exeter Analytical Inc. CE-440 microanalyzer. Infrared spectra were collected on an FTIR spectrometer Nicolet Nexus-470. Stille coupling and Suzuki–Miyaura reactions mixture were analyzed by gas–liquid chromatography using a Shimadzu GC-14B instrument equipped with a flame-ionization detector and a HP-5MS column (30 m × 0.25 mm × 0.25 mm), using nitrogen as carrier gas. Mass spectra (EI) were obtained at 70 eV on a Hewlett Packard HP-5890 GC/MS instrument equipped with a HP-5972 selective mass detector.

The volatile compounds of the grilled primal goat meat cuts were determined using a solid-phase microextraction gas chromatography–mass spectrometry (SPME GC-MS) [2 (link)]. The minced meat (5 g) was placed in a 20 mL headspace vial. The vials were tightly capped with a PTFE septum and heated at 60 °C with an equilibrium time of 2 h. Then, volatiles were allowed to absorb into an SPME fiber (50/30 lm DVB/Carboxen™/PDMS StableFlex™) (Supelco, Bellefonte, PA, USA) at 60 °C for 1 h. After that, the SPME device was removed, and the samples were immediately inserted into the injection port of the GC-MS. An HP 5890 series II gas chromatography (GC) coupled with HP 5972 mass-selective detector equipped with a splitless injector and coupled with a quadrupole mass detector (Hewlett Packard, Atlanta, GA, USA) was used to separate and identify the volatiles. The compounds were identified using ChemStation Library Search (Wiley 275.L). Quantitative determination was evaluated using an internal calibration curve of the stock solutions of the compounds in ultra-pure water saturated in salt and analyzed by the optimized HS-SPME method, in which the quantification limits were calculated to a signal-to-noise (S/N) ratio of 10. The identified volatile compounds were presented as a percentage of the relative peak area of the total peak.