Gcms qp5050a mass spectrometer

The given extract was analyzed by GC–MS electron impact ionization (EI) method on GC-17A gas chromatograph (Shimadzu) coupled to a GC–MS QP 5050A Mass Spectrometer (Shimadzu). A fused silica capillary column (30 m × 2.5 mm; 0.25 mm film thickness), coated with DB-5 ms (J&W) was used. The following conditions were used for GC–MS run; Injection temperature: 300 °C, interface temperature: 300 °C, ion source was adjusted to 250 °C, carrier gas: helium (flow rate of 1 ml min⁻¹). The analysis was performed following temperature program: 1 min. of isothermal heating at 100 °C followed by heating at 300 °C for 20 min. The mass spectra were recorded at 2 scan sec-1 with a scanning range of 40–850 m/z. Each component was quantified based on peak areas and normalization based on the internal standard.

Then, the synthesis of BBHC was continued as described previously [23 (link)]. In a 50 mL SNRB flask, 2-benzoylcyclohexanone (5 mmol) and 3-bromo-4-hydroxybenzaldehyde (5 mmol) were dissolved in 30 mL of acetic acid. Catalytic amount of concentrated sulfuric acid was added and the reaction mixture was stirred overnight. The resulting mixture was extracted with ethyl acetate and washed with 10% sodium bicarbonate solution. The organic layer was then dried over anhydrous magnesium sulphate and evaporated using rotary evaporator (Rotavapor^®R-300System, Heidolph Instruments GmbH & CO. KG, Schwabach, Germany). The targeted compound was purified by column chromatography (Merck silica gel 60, mesh 70–230 and elution with 95% hexane: 5% ethyl acetate) to produce BBHC. The structure (Figure 6) and the purity of the compound were identified and characterized by using ¹H-NMR and ¹³C-NMR (Varian 500 MHz, Varian Inc., Palo Alto, CA, USA), HPLC utilizing Waters Xbridge C18 column (5 µm, 150 mm × 4.6 mm) (Thermo Finnigan Surveyor, San Josè, CA, USA) and gas chromatography mass spectrometry (Shimadzu GCMS-QP5050A Mass Spectrometer, Shimadzu, Kyoto, Japan). The purity of the compound was 98.85%.

All solvents, hydrazine hydrate, KOH were purchased from commercial sources. Hydrazine hydrate 64% (monohydrate) technical grade was used. Bis(2-chloroprop-2-en-1-yl)sulfide was obtained according to the procedure [30 (link),31 (link)]. The ¹H, ¹³C, and ¹⁵N NMR spectra were recorded in CDCl₃ solutions at room temperature on Bruker DPX-400 and AV-400 spectrometers (400.13, 100.61 and 40.56 MHz, respectively). ¹H, ¹³C, and ¹⁵N chemical shifts (δ in ppm) were measured with accuracy of 0.01, 0.02, and 0.1 ppm, respectively. The residual solvent peak, δ_H = 7.27 and δ_C = 77.16 for CDCl₃, δ_H = 2.50 and δ_C = 39.52 for DMSO-d₆, and signal of nitromethane (¹⁵N) were used as references. Coupling constants (J) are reported in Hertz (Hz). The multiplicity abbreviations used are: s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet; br, broad signal. Chromato-mass spectrometry analysis was performed on a Shimadzu GCMS-QP5050A mass spectrometer (EI ionization, 70 eV). The IR spectra of the compounds were recorded on a Varian 3100 FT-IR spectrometer with the sample in thin film or in KBr. Elemental analysis was performed on a Thermo Finnigan Flash series 1112 Elemental analyzer. Column chromatography was carried out on silica gel 60 (70–200 mesh; Merk).