Determination of cocaine and benzoylecgonine by derivatization with iodomethane-D3 or PFPA/HFIP in human blood and urine using GC/MS (EI or PCI mode).
A method for the simultaneous detection and quantification of cocaine and benzoylecgonine from human blood and urine has been developed. Cocaine and benzoylecgonine were extracted from blood and urine with solid-phase columns containing C18 packing material. Clean, emulsion-free extracts were obtained. The analytes were derivatized with PFPA/HFIP or iodomethane-D3. The underivatized cocaine and derivatized benzoylecgonine were determined by GC/MS with positive chemical ionization (PCI) and the selected ion monitoring mode. Benzoylecgonine was derivatized with iodomethane-D3 to cocaine-D3. Both derivatives were chromatographed on a CP-SIL 5 capillary column. The recovery of extraction was greater than 70%. The detection limit for the PFPA/HFIP derivatives (20 ng/mL) was better than that for iodomethane-D3 derivatives (40 ng/mL). The procedure is simple, rapid, and reproducible. Standard curves were linear and the procedure was suitable for routine analysis. Using fluorescence polarization immunoassay (TDx, Abbott) (cutoff 100 ng/mL), along with one of the GC/MS methods described, we found no false positive or false negative results.
Aderjan
R E
RE
Institute for Forensic Medicine, University of Heidelberg, F.R.G.
Schmitt
G
G
Wu
M
M
Meyer
C
C
D000433:1-Propanol / Q000737:chemistry; D003042:Cocaine / Q000031:analogs & derivatives* / Q000097:blood* / Q000652:urine*; D016231:Fluorescence Polarization Immunoassay; D005466:Fluorocarbons / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D006847:Hydrocarbons, Iodinated / Q000737:chemistry; D020005:Propanols; D015813:Substance Abuse Detection / Q000379:methods*; D006845:Hydrocarbons, Fluorinated
D000433:1-Propanol; D003042:Cocaine; D005466:Fluorocarbons; D006847:Hydrocarbons, Iodinated; D020005:Propanols; C068048:pentafluoropropionic anhydride; C001337:hexafluoroisopropanol; D006845:Hydrocarbons, Fluorinated; C005618:benzoylecgonine; C014055:methyl iodide