Evaluation of microextraction by packed sorbent, liquid-liquid microextraction and derivatization pretreatment of diet-derived phenolic acids in plasma by gas chromatography with triple quadrupole mass spectrometry.
Luis BustamanteDiana CárdenasDietrich von BaerEdgar PasteneDaniel Duran-SandovalCarola VergaraClaudia MardonesPublished in: Journal of separation science (2017)
Miniaturized sample pretreatments for the analysis of phenolic metabolites in plasma, involving protein precipitation, enzymatic deconjugation, extraction procedures, and different derivatization reactions were systematically evaluated. The analyses were conducted by gas chromatography with mass spectrometry for the evaluation of 40 diet-derived phenolic compounds. Enzyme purification was necessary for the phenolic deconjugation before extraction. Trimethylsilanization reagent and two different tetrabutylammonium salts for derivatization reactions were compared. The optimum reaction conditions were 50 μL of trimethylsilanization reagent at 90°C for 30 min, while tetrabutylammonium salts were associated with loss of sensitivity due to rapid activation of the inert gas chromatograph liner. Phenolic acids extractions from plasma were optimized. Optimal microextraction by packed sorbent performance was achieved using an octadecylsilyl packed bed and better recoveries for less polar compounds, such as methoxylated derivatives, were observed. Despite the low recovery for many analytes, repeatability using an automated extraction procedure in the gas chromatograph inlet was 2.5%. Instead, using liquid-liquid microextraction, better recoveries (80-110%) for all analytes were observed at the expense of repeatability (3.8-18.4%). The phenolic compounds in gerbil plasma samples, collected before and 4 h after the administration of a calafate extract, were analyzed with the optimized methodology.
Keyphrases
- gas chromatography
- mass spectrometry
- tandem mass spectrometry
- liquid chromatography
- high resolution mass spectrometry
- solid phase extraction
- high performance liquid chromatography
- gas chromatography mass spectrometry
- ultra high performance liquid chromatography
- simultaneous determination
- ionic liquid
- capillary electrophoresis
- high resolution
- liquid chromatography tandem mass spectrometry
- ms ms
- weight loss
- oxidative stress
- molecularly imprinted
- room temperature
- hydrogen peroxide
- carbon dioxide
- blood brain barrier
- binding protein