PMID- 27108048 OWN - NLM STAT- MEDLINE DCOM- 20161214 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1447 DP - 2016 May 20 TI - Determination of amphetamines in hair by integrating sample disruption, clean-up and solid phase derivatization. PG - 47-56 LID - S0021-9673(16)30459-9 [pii] LID - 10.1016/j.chroma.2016.04.036 [doi] AB - The utility of matrix solid phase dispersion (MSPD) for the direct analysis of amphetamines in hair samples has been evaluated, using liquid chromatography (LC) with fluorescence detection and precolumn derivatization. The proposed approach is based on the employment of MSPD for matrix disruption and clean-up, followed by the derivatization of the analytes onto the dispersant-sample blend. The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) has been used for derivatization. Different conditions for MSPD, analyte purification and solid phase derivatization have been tested, using amphetamine (AMP), methamphetamine (MET), ephedrine (EPE) and 3,4-methylenedioxymethamphetamine (MDMA) as model compounds. The results have been compared with those achieved by using ultrasound-assisted alkaline digestion and by MSPD combined with conventional solution derivatization. On the basis of the results obtained, a methodology is proposed for the analysis of amphetamines in hair which integrates sample disruption, clean-up and derivatization using a C18 phase. Improved sensitivity is achieved with respect to that obtained by the alkaline digestion or by the MSPD followed by solution derivatization methods. The method can be used for the quantification of the tested amphetamines within the 2.0-20.0ng/mg concentration interval, with limits of detection (LODs) of 0.25-0.75ng/mg. The methodology is very simple and rapid (the preparation of the sample takes less than 15min). CI - Copyright (c) 2016 Elsevier B.V. All rights reserved. FAU - Argente-Garcia, A AU - Argente-Garcia A AD - Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100-Burjassot, Valencia, Spain. FAU - Moliner-Martinez, Y AU - Moliner-Martinez Y AD - Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100-Burjassot, Valencia, Spain. FAU - Campins-Falco, P AU - Campins-Falco P AD - Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100-Burjassot, Valencia, Spain. FAU - Verdu-Andres, J AU - Verdu-Andres J AD - Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100-Burjassot, Valencia, Spain. FAU - Herraez-Hernandez, R AU - Herraez-Hernandez R AD - Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100-Burjassot, Valencia, Spain. Electronic address: rosa.herraez@uv.es. LA - eng PT - Journal Article DEP - 20160420 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Amphetamines) RN - 0 (Fluorenes) RN - 0 (Fluorescent Dyes) RN - 44RAL3456C (Methamphetamine) RN - 9PLB0BTT90 (1-(9-fluorenyl)methyl chloroformate) RN - CK833KGX7E (Amphetamine) RN - GN83C131XS (Ephedrine) RN - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine) SB - IM MH - Amphetamine/analysis MH - Amphetamines/*analysis MH - Chromatography, Liquid/methods MH - Ephedrine/analysis MH - Fluorenes/chemistry MH - Fluorescent Dyes/chemistry MH - Hair/*chemistry MH - Humans MH - Methamphetamine/analysis MH - N-Methyl-3,4-methylenedioxyamphetamine/analysis OTO - NOTNLM OT - Amphetamines OT - Drug analysis OT - Hair OT - Liquid chromatography OT - Matrix-solid phase dispersion (MSPD) OT - Solid phase derivatization EDAT- 2016/04/25 06:00 MHDA- 2016/12/15 06:00 CRDT- 2016/04/25 06:00 PHST- 2016/02/23 00:00 [received] PHST- 2016/04/14 00:00 [revised] PHST- 2016/04/14 00:00 [accepted] PHST- 2016/04/25 06:00 [entrez] PHST- 2016/04/25 06:00 [pubmed] PHST- 2016/12/15 06:00 [medline] AID - S0021-9673(16)30459-9 [pii] AID - 10.1016/j.chroma.2016.04.036 [doi] PST - ppublish SO - J Chromatogr A. 2016 May 20;1447:47-56. doi: 10.1016/j.chroma.2016.04.036. Epub 2016 Apr 20.