TY - JOUR
T1 - Electromembrane extraction of stimulating drugs from undiluted whole blood
AU - Jamt, Ragnhild Elén Gjulem
AU - Gjelstad, Astrid
AU - Eibak, Lars Erik Eng
AU - Øiestad, Elisabeth Leere
AU - Christophersen, Asbjørg Solberg
AU - Rasmussen, Knut Einar
AU - Pedersen-Bjergaard, Stig
N1 - Copyright © 2011 Elsevier B.V. All rights reserved.
PY - 2012/4/6
Y1 - 2012/4/6
N2 - For the first time, electromembrane extraction (EME) of six basic drugs of abuse from undiluted whole blood and post mortem blood in a totally stagnant system is reported. Cathinone, methamphetamine, 3,4-methylenedioxy-amphetamine (MDA), 3,4-methylenedioxy-methamphet-amine (MDMA), ketamine and 2,5-dimethoxy-4-iodoamphetamine (DOI) were extracted from the whole blood sample, through a supported liquid membrane (SLM) consisting of 1-ethyl-2-nitrobenzene (ENB) immobilized in the pores of a hollow fiber, and into an aqueous acceptor solution inside the lumen of the hollow fiber. The SLM acts as a barrier with efficient exclusion of all macromolecules and acidic substances in the sample. Due to the application of the electrical field, only the cationic compounds of interest are extracted efficiently across the membrane, thus providing extremely clean extracts for analysis with liquid chromatography-mass spectrometry, LC-MS. Recoveries in the range 10-30% were obtained from 80 µl whole blood within 5 min extraction time and an applied voltage of 15V across the SLM. The optimized technique was tested on real forensic whole blood samples taken from three forensic autopsy cases and on five forensic whole blood samples from living persons. The results were in agreement with the analysis using standard sample preparation methods (liquid-liquid extraction) performed on the same samples by Norwegian Institute of Public Health (NIPH), Division of Forensic Toxicology and Drug Abuse Research. Evaluation data were acceptable, with limit of detections (LODs) in the range 40-2610 pg/mL, well below concentrations associated with drug abuse; linearites in the range between 10 and 250 ng/mL with r(2) values above 0.9939, and with repeatability (RSD) of 7-32%.
AB - For the first time, electromembrane extraction (EME) of six basic drugs of abuse from undiluted whole blood and post mortem blood in a totally stagnant system is reported. Cathinone, methamphetamine, 3,4-methylenedioxy-amphetamine (MDA), 3,4-methylenedioxy-methamphet-amine (MDMA), ketamine and 2,5-dimethoxy-4-iodoamphetamine (DOI) were extracted from the whole blood sample, through a supported liquid membrane (SLM) consisting of 1-ethyl-2-nitrobenzene (ENB) immobilized in the pores of a hollow fiber, and into an aqueous acceptor solution inside the lumen of the hollow fiber. The SLM acts as a barrier with efficient exclusion of all macromolecules and acidic substances in the sample. Due to the application of the electrical field, only the cationic compounds of interest are extracted efficiently across the membrane, thus providing extremely clean extracts for analysis with liquid chromatography-mass spectrometry, LC-MS. Recoveries in the range 10-30% were obtained from 80 µl whole blood within 5 min extraction time and an applied voltage of 15V across the SLM. The optimized technique was tested on real forensic whole blood samples taken from three forensic autopsy cases and on five forensic whole blood samples from living persons. The results were in agreement with the analysis using standard sample preparation methods (liquid-liquid extraction) performed on the same samples by Norwegian Institute of Public Health (NIPH), Division of Forensic Toxicology and Drug Abuse Research. Evaluation data were acceptable, with limit of detections (LODs) in the range 40-2610 pg/mL, well below concentrations associated with drug abuse; linearites in the range between 10 and 250 ng/mL with r(2) values above 0.9939, and with repeatability (RSD) of 7-32%.
KW - Alkaloids
KW - Amphetamines
KW - Chemical Fractionation
KW - Chromatography, High Pressure Liquid
KW - Electrochemical Techniques
KW - Equipment Design
KW - Forensic Medicine
KW - Humans
KW - Ketamine
KW - Limit of Detection
KW - Membranes, Artificial
KW - Reproducibility of Results
KW - Street Drugs
KW - Tandem Mass Spectrometry
U2 - 10.1016/j.chroma.2011.08.058
DO - 10.1016/j.chroma.2011.08.058
M3 - Journal article
C2 - 21899849
SN - 0301-4770
VL - 1232
SP - 27
EP - 36
JO - Journal of Chromatography
JF - Journal of Chromatography
ER -
