Identification and quantitation of phosphatidylethanols in oral fluid by liquid chromatography-tandem mass spectrometry.

作者: Shahid Ullah , Anders Helander , Olof Beck

DOI: 10.1515/CCLM-2016-0752

关键词:

摘要: Background Phosphatidylethanols (PEth) are formed from phosphatidylcholines and ethanol used as a specific sensitive alcohol biomarker. An analytical method for analysis of PEth in oral fluid based on high-performance liquid chromatography coupled to quadrupole tandem mass spectrometer (LC-MS/MS) was developed validated applied samples collected patients undergoing detoxification. Methods A 200-μL aliquot fluid, using the QuantisalTM device, extracted with chloroform/methanol containing internal standard subjected LC-MS/MS three selected forms (16:0/16:0, 16:0/18:1, 16:0/18:2). Chromatographic separation achieved UPLC BEH phenyl column, mobile phase consisting acetonitrile water 10 mmol/L ammonium hydrogen carbonate 0.1% ammonia. The MS instrument operated negative electrospray ionization reaction monitoring mode. Results detection limit 16:0/16:0, 16:0/18:2 ~0.1 ng/mL, extraction recoveries at 2.0 ng/mL were range 99%-114%. Method linearity over concentration up 200 ≥0.99. No significant deviation results observed an analyte stability study two different concentrations temperatures 3 months. In 35 detoxification, highest 16:0/18:1 (Detected range, 0.51-55.3 ng/mL; mean, 8.5; median, 3.1). addition, all variably identified majority (63%) samples. values showed weak positive correlation corresponding whole blood (r=0.50, p=0.026, n=20). Conclusions could reliably detect quantify after exposure. characterized by validation data satisfactory recovery, sensitivity, accuracy, imprecision, clinical suggest that measurement can be biomarker consumption, such non-invasive complement blood. However, further studies required evaluate test characteristics (e.g. sensitivity half-life) comparison

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