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

VL - 1232

SP - 27

EP - 36

JO - Journal of Chromatography

JF - Journal of Chromatography

SN - 0301-4770

ER -