作者: Shahid Ullah , Sören Sandqvist , Olof Beck
DOI: 10.1021/ACS.ANALCHEM.5B03433
关键词:
摘要: An analytical method based on high-performance liquid chromatography coupled to quadrupole tandem mass spectrometry was developed for the quantitative determination of four phosphatidylcholines (PCs) in human exhaled breath particles. Analytes were conveniently collected an electrostatic polymer filter and extracted with methanol prior analysis. Chromatographic separation performed ultraperformance chromatographic ethylene bridged hybrid phenyl column using a mobile phase consisting water containing 4 mM ammonium formate 0.1% ammonia. The spectrometer operated positive electrospray ionization selected reaction monitoring mode. Detection limits PC 16:0/16:0 (dipalmitoylphosphatidylcholine, DPPC), 16:0/18:1, 16:0/18:2, 18:0/18:2 <0.01 ng/filter. Method recoveries at concentration levels 0.1 10 ng/filter 100-110% 101-121%, respectively. Acceptable precision coefficients variation <20% accuracies 100% ± 20% achieved. Identification individual PCs basis two product ions correct ion ratios retention times. highest amount found DPPC median 1.14 (range 0.6-21 ng/filter), molar DPPC/PC (16:0/18:1) 1.98 0.48-2.75). A different pattern lower ratio (∼0.15) oral fluid. most significant element this study use precolumn LC system collecting particles electret filter. Due interference by background contamination, isolator (PFC kit) installed between eluent mixer injector reduce contamination. This is first LC/MS where successfully applied analyze simple convenient collection procedure.