PMID- 23141624
OWN - NLM
STAT- MEDLINE
DCOM- 20130422
LR  - 20191210
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1267
DP  - 2012 Dec 7
TI  - Dispersive liquid-liquid microextraction prior to field-amplified sample 
      injection for the sensitive analysis of 3,4-methylenedioxymethamphetamine, 
      phencyclidine and lysergic acid diethylamide by capillary electrophoresis in 
      human urine.
PG  - 189-97
LID - S0021-9673(12)01566-X [pii]
LID - 10.1016/j.chroma.2012.10.011 [doi]
AB  - A novel capillary zone electrophoresis (CZE) with ultraviolet detection method 
      has been developed and validated for the analysis of 
      3,4-methylenedioxymethamphetamine (MDMA), lysergic acid diethylamide (LSD) and 
      phencyclidine (PCP) in human urine. The separation of these three analytes has 
      been achieved in less than 8 min in a 72-cm effective length capillary with 50-mum 
      internal diameter. 100 mM NaH(2)PO(4)/Na(2)HPO(4), pH 6.0 has been employed as 
      running buffer, and the separation has been carried out at temperature and 
      voltage of 20 degrees C, and 25kV, respectively. The three drugs have been detected at 
      205 nm. Field amplified sample injection (FASI) has been employed for on-line 
      sample preconcentration. FASI basically consists in a mismatch between the 
      electric conductivity of the sample and that of the running buffer and it is 
      achieved by electrokinetically injecting the sample diluted in a solvent of lower 
      conductivity than that of the carrier electrolyte. Ultrapure water resulted to be 
      the better sample solvent to reach the greatest enhancement factor. Injection 
      voltage and time have been optimized to 5 kV and 20s, respectively. The 
      irreproducibility associated to electrokinetic injection has been correcting by 
      using tetracaine as internal standard. Dispersive liquid-liquid microextraction 
      (DLLME) has been employed as sample treatment using experimental design and 
      response surface methodology for the optimization of critical variables. Linear 
      responses were found for MDMA, PCP and LSD in presence of urine matrix between 
      10.0 and 100 ng/mL approximately, and LODs of 1.00, 4.50, and 4.40 ng/mL were 
      calculated for MDMA, PCP and LSD, respectively. The method has been successfully 
      applied to the analysis of the three drugs of interest in human urine with 
      satisfactory recovery percentages.
CI  - Copyright (c) 2012 Elsevier B.V. All rights reserved.
FAU - Airado-Rodriguez, Diego
AU  - Airado-Rodriguez D
AD  - Department of Analytical Chemistry, Faculty of Sciences, University of Granada, 
      Granada, Spain.
FAU - Cruces-Blanco, Carmen
AU  - Cruces-Blanco C
FAU - Garcia-Campana, Ana M
AU  - Garcia-Campana AM
LA  - eng
PT  - Evaluation Study
PT  - Journal Article
DEP - 20121016
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 8NA5SWF92O (Lysergic Acid Diethylamide)
RN  - J1DOI7UV76 (Phencyclidine)
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
SB  - IM
MH  - Electrophoresis, Capillary/*methods
MH  - Humans
MH  - Liquid Phase Microextraction/*methods
MH  - Lysergic Acid Diethylamide/isolation & purification/*urine
MH  - N-Methyl-3,4-methylenedioxyamphetamine/isolation & purification/*urine
MH  - Phencyclidine/isolation & purification/*urine
EDAT- 2012/11/13 06:00
MHDA- 2013/04/23 06:00
CRDT- 2012/11/13 06:00
PHST- 2012/06/12 00:00 [received]
PHST- 2012/10/08 00:00 [revised]
PHST- 2012/10/09 00:00 [accepted]
PHST- 2012/11/13 06:00 [entrez]
PHST- 2012/11/13 06:00 [pubmed]
PHST- 2013/04/23 06:00 [medline]
AID - S0021-9673(12)01566-X [pii]
AID - 10.1016/j.chroma.2012.10.011 [doi]
PST - ppublish
SO  - J Chromatogr A. 2012 Dec 7;1267:189-97. doi: 10.1016/j.chroma.2012.10.011. Epub 
      2012 Oct 16.