Simultaneous determination of amphetamine-type stimulants and cannabinoids in fingernails by gas chromatography-mass spectrometry.
A gas chromatography-mass spectrometric (GC-MS) method was developed and validated for the simultaneous detection and quantification of four amphetamine-type stimulants (amphetamine (AP), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA)) and two cannabinoids (Delta9-tetrahydrocannabinol (Delta9-THC) and 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH)) in fingernails. Fingernail clippings (30 mg) were washed with distilled water and methanol, and then incubated in 1.0 M sodium hydroxide at 95 degrees C for 30 min. The compounds of interest were isolated by liquid-liquid extraction followed by derivatization with N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA) at 70 degrees C for 15 min. The derivatized compounds were analyzed by GC-MS in the selective ion monitoring (SIM) mode. The linear ranges were 0.1-15.0 ng/mg for AP, 0.2-15.0 ng/mg for MDA, Delta9-THC and THCCOOH, and 0.2-30.0 ng/mg for MA and MDMA, with good correlation coefficients (r2 > 0.9991). The intra-day, inter-day, and inter-person precisions were within 10.6%, 6.3%, and 5.3%, respectively. The intra-day, inter-day and inter-person accuracies were between -6.1 and 5.0%, -6.2 and 5.7%, and -6.4 and 5.6%, respectively. The limits of detection (LODs) and quantification (LOQs) for each compound were lower than 0.056 and 0.2 ng/mg, respectively. The recoveries were in the range of 74.0-94.8%. Positive GC-MS results were obtained from specimens of nine suspected MA or cannabis abusers. The concentration ranges of MA, AP, and THCCOOH were 0.10-1.41, 0.12-2.64, and 0.20 ng/mg, respectively. Based on these results, the method proved to be effective for the simultaneous qualification and quantification of amphetamine-type stimulants and cannabinoids in fingernails.
Kim
Jin Young
JY
Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, 706, Banporo, Seocho-gu, Seoul, 137-730, Korea. paxus@spo.go.kr
Cheong
Jae Chul
JC
Kim
Min Kyoung
MK
Lee
Jae Il
JI
In
Moon Kyo
MK
D015104:3,4-Methylenedioxyamphetamine / Q000032:analysis; D000661:Amphetamine / Q000032:analysis; D019969:Amphetamine-Related Disorders / Q000175:diagnosis* / Q000378:metabolism; D000662:Amphetamines / Q000032:analysis*; D013759:Dronabinol / Q000031:analogs & derivatives / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D002189:Marijuana Abuse / Q000175:diagnosis* / Q000378:metabolism; D008694:Methamphetamine / Q000032:analysis; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis; D009262:Nails / Q000737:chemistry*; D015588:Observer Variation; D015203:Reproducibility of Results; D015813:Substance Abuse Detection / Q000379:methods*
D000662:Amphetamines; D008694:Methamphetamine; D015104:3,4-Methylenedioxyamphetamine; C016780:11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid; D013759:Dronabinol; D000661:Amphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine