Comprehensive automation of the solid phase extraction gas chromatographic mass spectrometric analysis (SPE-GC/MS) of opioids, cocaine, and metabolites from serum and other matrices.
The analysis of opioids, cocaine, and metabolites from blood serum is a routine task in forensic laboratories. Commonly, the employed methods include many manual or partly automated steps like protein precipitation, dilution, solid phase extraction, evaporation, and derivatization preceding a gas chromatography (GC)/mass spectrometry (MS) or liquid chromatography (LC)/MS analysis. In this study, a comprehensively automated method was developed from a validated, partly automated routine method. This was possible by replicating method parameters on the automated system. Only marginal optimization of parameters was necessary. The automation relying on an x-y-z robot after manual protein precipitation includes the solid phase extraction, evaporation of the eluate, derivatization (silylation with N-methyl-N-trimethylsilyltrifluoroacetamide, MSTFA), and injection into a GC/MS. A quantitative analysis of almost 170 authentic serum samples and more than 50 authentic samples of other matrices like urine, different tissues, and heart blood on cocaine, benzoylecgonine, methadone, morphine, codeine, 6-monoacetylmorphine, dihydrocodeine, and 7-aminoflunitrazepam was conducted with both methods proving that the analytical results are equivalent even near the limits of quantification (low ng/ml range). To our best knowledge, this application is the first one reported in the literature employing this sample preparation system.
GERSTEL GmbH & Co. KG, Eberhard-Gerstel-Platz 1, 45473, Muelheim, Germany, oliver_lerch@gerstel.de.
Oliver
O
Lerch
Oliver
O
Temme
Thomas
T
Daldrup
D000081:Acetamides / Q000737:chemistry; D000701:Analgesics, Opioid / Q000032:analysis* / Q000097:blood / Q000652:urine; D001331:Automation; D003042:Cocaine / Q000032:analysis* / Q000097:blood / Q000652:urine; D003061:Codeine / Q000031:analogs & derivatives / Q000032:analysis / Q000097:blood / Q000652:urine; D005445:Flunitrazepam / Q000031:analogs & derivatives / Q000032:analysis / Q000097:blood / Q000652:urine; D005463:Fluoroacetates / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D008691:Methadone / Q000032:analysis / Q000097:blood / Q000652:urine; D009020:Morphine / Q000032:analysis / Q000097:blood / Q000652:urine; D009022:Morphine Derivatives / Q000032:analysis / Q000097:blood / Q000652:urine; D015203:Reproducibility of Results; D012371:Robotics / Q000295:instrumentation / Q000379:methods; D052616:Solid Phase Extraction / Q000379:methods*; D015813:Substance Abuse Detection / Q000379:methods*; D014297:Trimethylsilyl Compounds / Q000737:chemistry
D000081:Acetamides; D000701:Analgesics, Opioid; D005463:Fluoroacetates; D009022:Morphine Derivatives; D014297:Trimethylsilyl Compounds; C086665:N-methyl-N-(trimethylsilyl)trifluoroacetamide; D005445:Flunitrazepam; D009020:Morphine; C036343:7-aminoflunitrazepam; D003042:Cocaine; C026979:6-O-monoacetylmorphine; C014481:dihydrocodeine; D008691:Methadone; D003061:Codeine