Rapid and simple determination of psychotropic phenylalkylamine derivatives in human hair by gas chromatography-mass spectrometry using micro-pulverized extraction.
A gas chromatography-mass spectrometric (GC-MS) method was developed and validated for the determination of five psychotropic phenylalkylamine derivatives (amphetamine, AP; methamphetamine, MA; 3,4-methylenedioxyamphetamine, MDA; 3,4-methylenedioxymethamphetamine, MDMA; norketamine, NKT) in human hair. Hair samples (10mg) were washed with distilled water and acetone, mechanically pulverized for 1.5 min with a bead mill, and then incubated in 1 mL of methanol under ultrasonication at 50 degrees C for 1h. The resulting solutions were evaporated to dryness, derivatized using heptafluorobutyric anhydride (HFBA) at 50 degrees C for 30 min, and analyzed by GC-MS. The linear ranges were 0.1-20.0 ng/mg for AP and MA and 0.05-20.0 ng/mg for MDA, MDMA, and NKT, with the coefficients of determination (r(2)>0.9982). The intra-day and inter-day precisions were within 11.5% and 12.8%, respectively. The intra-day and inter-day accuracies were -4.1% to 5.8% and -6.6% to 4.2%, respectively. The limits of detections (LODs) for each compound were lower than 0.028 ng/mg. The recoveries were in the range of 78.9-101.2%. Based on these results, the method proved to be effective for the rapid and simple determination of phenylalkylamine derivatives in hair specimens.
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
Lee
Jae Il
JI
In
Moon Kyo
MK
D015104:3,4-Methylenedioxyamphetamine / Q000032:analysis; D000661:Amphetamine / Q000032:analysis; D053593:Forensic Toxicology; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D006213:Hallucinogens / Q000032:analysis*; D006801:Humans; D007649:Ketamine / Q000031:analogs & derivatives / Q000032:analysis; D057230:Limit of Detection; D008694:Methamphetamine / Q000032:analysis; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis; D015813:Substance Abuse Detection / Q000379:methods*
D006213:Hallucinogens; D008694:Methamphetamine; D015104:3,4-Methylenedioxyamphetamine; D007649:Ketamine; D000661:Amphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine; C033419:norketamine