The EI MS have been recorded having a ionization voltage of 70 eV along with a supply temperature of 230 C. The software MSD ChemStation for Windows was utilised for information acquisition. Linear retention indices had been calculated applying Kovats process by linear interpolation from a series of n alkanes. Additional chemical characterization was accomplished for 3 key compounds among the novel compounds. Considering the fact that most other compounds had been represented by 1% of all novel substances, we couldn’t obtain adequate extracts to unambiguously recognize all remaining compounds. We obtained CI MS that has a Hewlett Packard 5890A gasoline chromatograph equipped using a 2 m fused silica guard column as well as a 30 m ? 0. 32 mm analytical column, The capillary column was directly coupled to a triple quadrupole mass spectrometer, Injector and transfer line were kept at 280 C. Temperature was stored at 70 C for three min then elevated at 10 C min up to 310 C, exactly where it remained consistent for five min.
The CI mass spectra have been recorded while in the good mode utilizing ammonia like a reagent gas. For HRMS, an Agilent 6890 gas chromatograph was outfitted that has a 30 m analytical column, A split in jection port at 250 C was employed for sample SP600125 structure introduction having a split ratio of three.1. The temperature system was the exact same as for CI MS. The helium carrier gasoline was set to 1. 0 ml min flow rate, The transfer line was kept at 270 C. HRMS have been acquired using a JMS T100GC time of flight MS in EI mode at 70 eV and JEOL MassCenter workstation computer software. Source and transfer line temperature had been 200 C and 270 C, respectively, and detector voltage was set at 2100 V. The acquisition assortment was m z 41 to 600 with a spectrum recoding interval of 0. 4 s. The procedure was tuned with PFK to accomplish a reso lution of five,000 at m z 292. 9824, as well as mass accuracy across all suitable ions was greater than four mmu.
NMR analyses have been carried out buy inhibitor utilizing hexane extracts of a number of tens of 1000s of ants. The extracts have been purified making use of conditioned SiOH columns with distilled hexane and chloroform as respective eluents. The novel compounds have been eluted with chloroform, which was then evaporated as well as fraction reconstituted in hexane. After concentration to 50 ul, the fraction was chromatographed in excess of two. 0 g silica gel in twelve fractions of four ml every single, working with the following solvents. one hundred.0, one hundred.0, 50.1, 20.1, ten.one, five.one, 3.1, 1.one, 0.one hundred, 0.one hundred, 0.a hundred, 0.one hundred. The novel compounds had been uncovered solely inside the initially 100% dichloromethane fraction, exactly where the main compound had a concentration of 89%. NMR spectra have been recorded on the Varian INOVA 500 MHz instrument equipped that has a 3 mm ID PFG probe. The 1H and 13C chemical shifts have been referenced to solvent signal at H C 7. 27 77. 0 ppm relative to TMS. All 1D and 2D NMR measurements had been carried out employing typical Varian pulse sequences.