Individual hydrocarbons identified to be macrocyclic alkanes in a torbanite from the Sydney Basin(Australia)were successfully isolated from its extracts using preparative gas chromatography and analyzed by NMR.Saturat...Individual hydrocarbons identified to be macrocyclic alkanes in a torbanite from the Sydney Basin(Australia)were successfully isolated from its extracts using preparative gas chromatography and analyzed by NMR.Saturated cyclic structures were confirmed by single peaks in the NMR~1H and~(13)C spectra indicating single forms of H and C atoms exist in these biomarker molecules.This is consistent with the methylene unit in a ring system assignment of the macrocyclic alkanes and accounts for a formula of(CH2)n.The unusual molecular structures of these compounds are consistent with those that were identified from previous GC retention index data and co-injection with a standard supports the previous research.The mass spectral fragmentation behaviors of representative cyclic alkanes were further investigated by comparing them with the mass spectra of isolated individual macrocyclic alkanes.The characteristic fragment ions in the macrocyclic alkanes of(M–28)+and base peaks of m/z 97,111,125,etc.,can be assigned as being generated by simple a-/i-cleavage and hydrogen rearrangement.These fragmentation pathways combined with retention indices should assist in differentiating these compounds from monounsaturated alkenes and alkylated monocyclics having similar mass spectral characteristics in other geological samples.展开更多
Compositional data on the sterol and alcohol fractions isolated from deep-sea marine sediments from the Okinawa Trough were obtained to determine the relative contribution from. marine and terrestrial inputs. Followin...Compositional data on the sterol and alcohol fractions isolated from deep-sea marine sediments from the Okinawa Trough were obtained to determine the relative contribution from. marine and terrestrial inputs. Following extraction, the sterol plus alcohol fraction was isolated by layer chromatography, derivatized with BSTFA and then analysed by capillary GC and GC-MS. A suite of C26-C29 stenols and stanols and C30-C32 keto - alcohols were identified in the sediments. The thermal stability of the compounds in these sediments was studied by heating portions of the surface sediment in glass tubes fpr 16 hours at temperatures from 50℃ to 200℃.The C27 stanol/stenol ratio increased when temperatures went up to 175℃ , but the distribution of C30-C32 Keto - alcohols remained unaffected. At 200℃ most of the sterols and Keto - alcohols were destroyed.展开更多
基金the financial support from The Strategic Priority Research Program of the Chinese Academy of Sciences(XDA14010102)Chinese National Science Foundation grants(4197306941673045)。
文摘Individual hydrocarbons identified to be macrocyclic alkanes in a torbanite from the Sydney Basin(Australia)were successfully isolated from its extracts using preparative gas chromatography and analyzed by NMR.Saturated cyclic structures were confirmed by single peaks in the NMR~1H and~(13)C spectra indicating single forms of H and C atoms exist in these biomarker molecules.This is consistent with the methylene unit in a ring system assignment of the macrocyclic alkanes and accounts for a formula of(CH2)n.The unusual molecular structures of these compounds are consistent with those that were identified from previous GC retention index data and co-injection with a standard supports the previous research.The mass spectral fragmentation behaviors of representative cyclic alkanes were further investigated by comparing them with the mass spectra of isolated individual macrocyclic alkanes.The characteristic fragment ions in the macrocyclic alkanes of(M–28)+and base peaks of m/z 97,111,125,etc.,can be assigned as being generated by simple a-/i-cleavage and hydrogen rearrangement.These fragmentation pathways combined with retention indices should assist in differentiating these compounds from monounsaturated alkenes and alkylated monocyclics having similar mass spectral characteristics in other geological samples.
基金Supported by the National Natural Foundation of China
文摘Compositional data on the sterol and alcohol fractions isolated from deep-sea marine sediments from the Okinawa Trough were obtained to determine the relative contribution from. marine and terrestrial inputs. Following extraction, the sterol plus alcohol fraction was isolated by layer chromatography, derivatized with BSTFA and then analysed by capillary GC and GC-MS. A suite of C26-C29 stenols and stanols and C30-C32 keto - alcohols were identified in the sediments. The thermal stability of the compounds in these sediments was studied by heating portions of the surface sediment in glass tubes fpr 16 hours at temperatures from 50℃ to 200℃.The C27 stanol/stenol ratio increased when temperatures went up to 175℃ , but the distribution of C30-C32 Keto - alcohols remained unaffected. At 200℃ most of the sterols and Keto - alcohols were destroyed.
