The EI MS had been recorded that has a ionization voltage of 70 eV and a source temperature of 230 C. The application MSD ChemStation for Windows was utilised for data acquisition. Linear retention indices have been calculated working with Kovats process by linear interpolation from a series of n alkanes. Even more chemical characterization was completed for 3 major compounds amongst the novel compounds. Considering that most other compounds were represented by 1% of all novel substances, we could not acquire ample extracts to unambiguously identify all remaining compounds. We obtained CI MS with a Hewlett Packard 5890A gasoline chromatograph outfitted by using a 2 m fused silica guard column in addition to a 30 m ? 0. 32 mm analytical column, The capillary column was directly coupled to a triple quadrupole mass spectrometer, Injector and transfer line have been kept at 280 C. Temperature was kept at 70 C for three min and after that improved at ten C min as much as 310 C, exactly where it remained continual for five min.
The CI mass spectra were recorded while in the beneficial mode using ammonia like a reagent fuel. For HRMS, an Agilent 6890 gasoline chromatograph was outfitted having a thirty m analytical column, A split in jection port at 250 C was utilized for sample selleckchem GSK256066 introduction by using a split ratio of 3.one. The temperature plan was the exact same as for CI MS. The helium carrier gasoline was set to one. 0 ml min movement fee, The transfer line was kept at 270 C. HRMS had been acquired utilizing a JMS T100GC time of flight MS in EI mode at 70 eV and JEOL MassCenter workstation software package. Supply and transfer line temperature were 200 C and 270 C, respectively, and detector voltage was set at 2100 V. The acquisition assortment was m z 41 to 600 using a spectrum recoding interval of 0. four s. The procedure was tuned with PFK to realize a reso lution of five,000 at m z 292. 9824, and the mass accuracy across all suitable ions was better than four mmu.
NMR analyses had been performed selelck kinase inhibitor employing hexane extracts of many tens of a large number of ants. The extracts had been purified employing 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 the fraction reconstituted in hexane. Right after concentration to 50 ul, the fraction was chromatographed in excess of two. 0 g silica gel in twelve fractions of 4 ml just about every, making use of the following solvents. 100.0, a hundred.0, 50.1, twenty.one, ten.one, five.one, three.1, 1.one, 0.100, 0.100, 0.a hundred, 0.100. The novel compounds have been discovered solely during the 1st 100% dichloromethane fraction, in which the primary compound had a concentration of 89%. NMR spectra have been recorded on the Varian INOVA 500 MHz instrument equipped which has a 3 mm ID PFG probe. The 1H and 13C chemical shifts were 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 working with standard Varian pulse sequences.