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Liquid chromatography/time-of-flight mass spectrometry analysis of postmortem blood samples for targeted toxicological screening
Natl Board Forens Med, Dept Forens Genet and Forens Toxicol, S-58758 Linkoping, Sweden .
Natl Board Forens Med, Dept Forens Genet and Forens Toxicol, S-58758 Linkoping, Sweden .
Natl Board Forens Med, Dept Forens Genet and Forens Toxicol, S-58758 Linkoping, Sweden .
Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology. Linköping, .
2013 (English)In: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 405, no 12, 4107-4125 p.Article in journal (Refereed) Published
Abstract [en]

A liquid chromatography/time-of-flight mass spectrometry (LC-TOF-MS) method for targeted toxicological screening in human postmortem blood samples from forensic autopsy cases has been developed, validated and compared with a previously used method using gas chromatography with nitrogen-phosphorus detection (GC-NPD). Separation was achieved within 12 min by high-resolution gradient chromatography. Ions were generated in positive and negative electrospray ionization mode and were detected in 2-GHz single mass spectrometry mode, m/z range 50-1,000. Before injection, 0.25 g blood was prepared by protein precipitation with 500 mu L of a mixture of acetonitrile and ethanol containing deuterated internal standards. An in-house database comprising 240 drugs and metabolites was built by analysing solutions from certified standards or other documented reference material available. Identification was based on scoring of retention time, accurate mass measurement and isotopic pattern. Validation was performed on spiked blood samples and authentic postmortem blood samples. The thresholds defined as minimum required performance levels were for most compounds in the range from 0.01 to 0.10 mu g/g. Typically, a mass error of less than 2 ppm and a precision of area measurements of less than 5 % coefficient of variation were achieved. Positive identification was confirmed at concentrations up to 500 mu g/g. Most compounds were determined in positive ionization mode, but for a limited number of compounds (fewer than 4 %) negative ionization was needed and a few early-eluted compounds could not be identified owing to substantial influence of interferences from the matrix and were thus not included in the screening. A robust and valid toxicological screening by LC-TOF-MS for postmortem blood samples, covering 50 % more compounds, and with higher precision and sensitivity than the previously used screening by GC-NPD was achieved.

Place, publisher, year, edition, pages
Springer Verlag (Germany) , 2013. Vol. 405, no 12, 4107-4125 p.
Keyword [en]
Postmortem, Blood, Liquid chromatography, Mass spectrometry, Time of flight, Liquid chromatography/time-of-flight mass spectrometry
National Category
Engineering and Technology
URN: urn:nbn:se:liu:diva-93975DOI: 10.1007/s00216-013-6798-0ISI: 000317643900023OAI: diva2:628259
Available from: 2013-06-13 Created: 2013-06-13 Last updated: 2013-06-13

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Josefsson, Martin
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Department of Physics, Chemistry and BiologyThe Institute of Technology
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