Determination of amphetamine-type stimulants, ketamine and metabolites in fingernails by gas chromatography-mass spectrometry.
A gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the simultaneous qualification and quantification of methamphetamine (MA), amphetamine (AP), 3,4-methylenedioxy-N-methylamphetamine (MDMA), 3,4-methylenedioxy-N-amphetamine (MDA), ketamine (KET) and norketamine (NKT) in fingernails. Fingernail samples (20mg) were washed with distilled water and methanol, digested with 1.0M sodium hydroxide at 95 degrees C for 30 min, and then extracted with ethyl acetate. Extract solutions were evaporated to dryness, derivatized using heptafluorobutyric anhydride (HFBA) at 60 degrees C for 30 min, and analyzed by GC-MS. The linear ranges were 0.1-20.0 ng/mg for AP, MDMA and NKT, 0.2-20.0 ng/mg for MA and MDA, and 0.4-20.0 ng/mg for KET, with the coefficients of determination (r(2)>or=0.9989). The intra- and inter-day precisions were within 7.1% and 10.6%, respectively. The intra- and inter-day accuracies were -10.9% to 0.8% and -4.3% to 4.5%, respectively. The limits of detections (LODs) and the limits of quantifications (LOQs) for each analyte were lower than 0.094 ng/mg and 0.314 ng/mg, respectively. The recoveries were in the range of 72.3-94.9%. The average fingernail growth rates of two subjects for three years and six subjects for two months were 3.12 mm/month and 3.16 mm/month, respectively. The method proved to be suitable also for the simultaneous detection and quantification of MA, MDMA, KET and their metabolites in fingernails.
Kim
Jin Young
JY
Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, Seoul, Republic of Korea. paxus@spo.go.kr
Shin
Soon Ho
SH
In
Moon Kyo
MK
D000662:Amphetamines / Q000032:analysis*; D000700:Analgesics / Q000032:analysis*; D053593:Forensic Toxicology / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D007649:Ketamine / Q000031:analogs & derivatives / Q000032:analysis*; D009262:Nails / Q000737:chemistry* / Q000254:growth & development; D015813:Substance Abuse Detection / Q000379:methods
D000662:Amphetamines; D000700:Analgesics; D007649:Ketamine; C033419:norketamine