PubMed · 12933967
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G B Hart, M B Strauss. 2003-08-21. Hyperbaric oxygen therapy.. https://doi.org/10.1161/01.str.0000087115.91721.6e
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Triacylglycerols (TGs) and diacylglycerols (DGs) in 16 plant oil samples (hazelnut, pistachio, poppy-seed, almond, palm, Brazil-nut, rapeseed, macadamia, soyabean, sunflower, linseed, Dracocephalum moldavica, evening primrose, corn, amaranth, Silybum arianum) were analyzed by HPLC-MS with atmospheric pressure chemical ionization (APCI) and UV detection at 205 nm on two Nova-Pak C18 chromatographic columns connected in series. A single chromatographic column and non-aqueous ethanol-acetonitrile gradient system was used as a compromise between the analysis time and the resolution for the characterization of TG composition of five plant oils. APCI mass spectra were applied for the identification of all TGs and other acylglycerols. The isobaric positional isomers can be distinguished on the basis of different relative abundances of the fragment ions formed by preferred losses of the fatty acid from sn-1(3) positions compared to the sn-2 position. Excellent chromatographic resolution and broad retention window together with APCI mass spectra enabled positive identification of TGs containing fatty acids with odd numbers of carbon atoms such as margaric (C17:0) and heptadecanoic (C17:1) acids. The general fragmentation patterns of TGs in both APCI and electrospray ionization mass spectra were proposed on the basis of MSn spectra measured with an ion trap analyzer. The relative concentrations of particular TGs in the analyzed plant oils were estimated on the basis of relative peak areas measured with UV detection at 205 nm.
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A sensitive analytical method has been developed for identification of ubiquinones (UQ-n(Hx)) and menaquinones (MK-n(Hx)) in activated sludge by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry in negative mode (LC-NI-APCI-MS). Extraction and clean-up of samples were carried out on Sep-Pak Plus Silica solid-phase extraction cartridges. Complete separation of quinones was achieved with an ODS analytical column and using isopropyl ether-methanol (17:83, v/v) as the mobile phase. The compositions of ubiquinones and menaquinones were determined directly using combined information on retention time, the molecular ion mass and fragment ion masses. The lowest instrument quantitative detection limits (LODinst) for UQ-6, UQ-10, and Vitamin K1 were estimated to be 0.4, 4 and 0.12 ng (S/N = 10) using LC-NI-APCI-MS in SIM mode, and the lowest method detection limits (LODmeth) achieved by spiking experiment were estimated to be 0.2, 2 and 0.06 microg/g for UQ-6, UQ-10 and Vitamin K1, respectively. On the other hand, the LODinst for UQ-6, UQ-10, and Vitamin K1 were estimated to be 10, 100 and 2 ng (S/N = 10) using LC-NI-APCI-MS in full-scan mode, and the LODmeth were estimated to be 7, 60 and 1.2 microg/g for UQ-6, UQ-10, and Vitamin K1, respectively. Both LC-NI-APCI-MS and LC-UV/DAD were applied in the analysis of an activated sludge extract. UQ-n (n = 6-10), MK-n (n = 6-10), MK-n(H2) (n = 7-10), MK-n(H4) (n = 8-9) and MK-8(H6) were detected by LC-NI-APCI-MS, while UQ-6, UQ-7, MK-7(H), MK-9 and MK-10(H2) were not found by LC-UV/DAD. These results suggest that LC-NI-APCI-MS is more sensitive than LC-UV/DAD for the analysis of quinones in environmental samples such as sediment, activated sludge and bio-film in biological processes and other aquatic environments.