Gcmate mass spectrometer

All melting points were uncorrected. The progression of all the reactions was monitored by thin layer chromatography (TLC) using hexanes/ethyl acetate mixture as eluent. Column chromatography was carried out on silica gel by using increasing polarity. ¹H, ¹³C and DEPT-135 spectra were recorded in CDCl₃ using TMS as an internal standard on a Bruker 300 MHz spectrometer at room temperature. Chemical shift values were quoted in parts per million (ppm) and coupling constants (J) were quoted in Hertz (Hz). Mass spectra were recorded on JEOL GC mate mass spectrometer. The X-ray diffraction measurements were carried out at 298 K on a Bruker (2008) SMART APEX 2 area detector diffractometer (S1 File).

The IR spectral studies for both free diosmin and its metal complex were performed in solid state as pressed KBr pellets using a Perkin-Elmer FT-IR spectrophotometer (400–4000 cm¹). Jeol Gc-mate mass spectrometer was used to obtain the mass spectrum of the complex. The ¹H NMR and ¹³C NMR of diosmin as well as its complex were obtained at 300 MHz and 500 MHz, respectively, using a Bruker AM-500 instrument. The spectral analysis data were recorded without any modification for instrumental characteristics.

Gas chromatography coupled to a JEOL GCmate mass spectrometer operating in electron ionization (EI) mode were used for component analyses. Mass spectra were acquired scanning from m/z 20 to m/z 250. The constituents of the oils were identified by using standard reference compounds and also by matching the mass spectra fragmentation pattern with NIST Mass Spectra Library in the GC-MS database.