A validated positive chemical ionization GC/MS method for the identification and quantification of amphetamine, opiates, cocaine, and metabolites in human postmortem brain

被引:17
作者
Lowe, RH
Barnes, AJ
Lehrmann, E
Freed, WJ
Kleinman, JE
Hyde, TM
Herman, MM
Huestis, MA
机构
[1] NIDA, Chem & Drug Metab Sect, Intramural Res Program, NIH,DHHS, Baltimore, MD 21224 USA
[2] NIDA, Cellular Neurobiol Res Branch, Intramural Res Program, NIH,DHHS, Baltimore, MD 21224 USA
[3] NIMH, Clin Brain Disorders Branch, NIH, DHHS, Bethesda, MD 20892 USA
来源
JOURNAL OF MASS SPECTROMETRY | 2006年 / 41卷 / 02期
关键词
drugs of abuse; GC/MS; brain; cocaine; opiates;
D O I
10.1002/jms.975
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A sensitive and specific method for the simultaneous detection and quantification of amphetamine, opiates, and cocaine and metabolites in human postmortem brain was developed and validated. Analytes of interest included amphetamine, morphine, codeine, 6-acetylmorphine, cocaine, benzoylecgonine, ecgonine methyl ester, ecgonine ethyl ester, cocaethylene, and anhydroecgonine methyl ester. The method employed ultrasonic homogenization of brain tissue in pH 4.0 sodium acetate buffer and solid phase extraction. Extracts were derivatized with N-methyl-N-(tert-butyldimethylsilyl) trifluoroacetamide and N,O-bis(trimethylsilyl) trifluoroacetamide. Separation and quantification were accomplished on a bench-top positive chemical ionization capillary gas chromatograph/mass spectrometer with selected ion monitoring. Eight deuterated analogs were used as internal standards. Limits of quantification were 50 ng/g of brain. Calibration curves were linear to 1000 ng/g for anhydroecgonine methyl ester and 6-acetylmorphine, and to 2000 ng/g for all other analytes. Accuracy across the linear range of the assay ranged from 90.2 to 112.2%, and precision, as percent relative standard deviation, was less than 16.6%. Quantification of drug concentrations in brain is a useful research tool in neurobiology and in forensic and postmortem toxicology, identifying the type, relative magnitude, and recency of abused drug exposure. This method will be employed to quantify drug concentrations in human postmortem brain in support of basic and clinical research on the physiologic, biochemical, and behavioral effects of drugs in humans. Copyright (c) 2005 John Wiley & Sons, Ltd.
引用
收藏
页码:175 / 184
页数:10
相关论文
共 29 条
[1]   GAS CHROMATOGRAPHY-CHEMICAL IONIZATION MASS-SPECTROMETRY OF COCAINE AND ITS METABOLITES IN BIOLOGICAL-FLUIDS [J].
CHINN, DM ;
CROUCH, DJ ;
PEAT, MA ;
FINKLE, BS ;
JENNISON, TA .
JOURNAL OF ANALYTICAL TOXICOLOGY, 1980, 4 (01) :37-42
[2]   Generic fast gradient liquid chromatography/tandem mass spectrometry techniques for the assessment of the in vitro permeability across the blood-brain barrier in drug discovery [J].
Chu, I ;
Liu, F ;
Soares, A ;
Kumari, P ;
Nomeir, AA .
RAPID COMMUNICATIONS IN MASS SPECTROMETRY, 2002, 16 (15) :1501-1505
[3]   Studies on hydrolytic and oxidative metabolic pathways of anhydroecgonine methyl ester (methylecgonidine) using microsomal preparations from rat organs [J].
Fandiño, AS ;
Toennes, SW ;
Kauert, GF .
CHEMICAL RESEARCH IN TOXICOLOGY, 2002, 15 (12) :1543-1548
[4]   An unusual multiple drug intoxication case involving citalopram [J].
Fu, K ;
Konrad, RJ ;
Hardy, RW ;
Brissie, RM ;
Robinson, CA .
JOURNAL OF ANALYTICAL TOXICOLOGY, 2000, 24 (07) :648-650
[5]   A fatal overdose of cocaine associated with coingestion of marijuana, buprenorphine, and fluoxetine. Body fluid and tissue distribution of cocaine and its metabolites determined by hydrophilic interaction chromatography-mass spectrometry (HILIC-MS) [J].
Giroud, C ;
Michaud, K ;
Sporkert, F ;
Eap, C ;
Augsburger, M ;
Cardinal, P ;
Mangin, P .
JOURNAL OF ANALYTICAL TOXICOLOGY, 2004, 28 (06) :464-474
[6]   DISPOSITION OF HEROIN AND ITS METABOLITES IN HEROIN-RELATED DEATHS [J].
GOLDBERGER, BA ;
CONE, EJ ;
GRANT, TM ;
CAPLAN, YH ;
LEVINE, BS ;
SMIALEK, JE .
JOURNAL OF ANALYTICAL TOXICOLOGY, 1994, 18 (01) :22-28
[7]   ANALYSIS OF COCAINE AND METABOLITES IN BRAIN USING SOLID-PHASE EXTRACTION AND FULL-SCANNING GAS-CHROMATOGRAPHY ION-TRAP MASS-SPECTROMETRY [J].
HERNANDEZ, A ;
ANDOLLO, W ;
HEARN, WL .
FORENSIC SCIENCE INTERNATIONAL, 1994, 65 (03) :149-156
[8]   ANALYSIS OF COCAINE AND COCAETHYLENE IN BLOOD AND TISSUES BY GC-NPD AND GC-ION TRAP MASS-SPECTROMETRY [J].
HIME, GW ;
HEARN, WL ;
ROSE, S ;
COFINO, J .
JOURNAL OF ANALYTICAL TOXICOLOGY, 1991, 15 (05) :241-245
[9]   Sweat testing for cocaine, codeine and metabolites by gas chromatography - mass spectrometry [J].
Huestis, MA ;
Oyler, JM ;
Cone, EJ ;
Wstadik, AT ;
Schoendorfer, D ;
Joseph, RE .
JOURNAL OF CHROMATOGRAPHY B, 1999, 733 (1-2) :247-264
[10]  
Kalasinsky KS, 2001, J FORENSIC SCI, V46, P728