PMID- 20113714
OWN - NLM
STAT- MEDLINE
DCOM- 20100331
LR  - 20100201
IS  - 1873-4324 (Electronic)
IS  - 0003-2670 (Linking)
VI  - 661
IP  - 1
DP  - 2010 Feb 19
TI  - Monolithic silica spin column extraction and simultaneous derivatization of 
      amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas 
      chromatographic-mass spectrometric detection.
PG  - 42-6
LID - 10.1016/j.aca.2009.12.013 [doi]
AB  - A simple, sensitive, and specific method with gas chromatography-mass 
      spectrometry was developed for simultaneous extraction and derivatization of 
      amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by 
      using a monolithic silica spin column. All the procedures, such as sample 
      loading, washing, and elution were performed by centrifugation. APs and MDAs in 
      urine were adsorbed on the monolithic silica and derivatized with propyl 
      chloroformate in the column. Methamphetamine-d(5) was used as an internal 
      standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) 
      and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for 
      amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of 
      correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and 
      the relative standard deviation of the intra- and interday reproducibility for 
      urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged 
      from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) 
      in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The 
      proposed method can be used to perform simultaneous extraction and derivatization 
      on spin columns that have been loaded with a small quantity of solvent by using 
      centrifugation.
CI  - Copyright 2009 Elsevier B.V. All rights reserved.
FAU - Nakamoto, Akihiro
AU  - Nakamoto A
AD  - Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, 
      Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825, Japan.
FAU - Nishida, Manami
AU  - Nishida M
FAU - Saito, Takeshi
AU  - Saito T
FAU - Kishiyama, Izumi
AU  - Kishiyama I
FAU - Miyazaki, Shota
AU  - Miyazaki S
FAU - Murakami, Katsunori
AU  - Murakami K
FAU - Nagao, Masataka
AU  - Nagao M
FAU - Namura, Akira
AU  - Namura A
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20091216
PL  - Netherlands
TA  - Anal Chim Acta
JT  - Analytica chimica acta
JID - 0370534
RN  - 0 (Amphetamines)
RN  - 4764-17-4 (3,4-Methylenedioxyamphetamine)
RN  - 7631-86-9 (Silicon Dioxide)
SB  - IM
MH  - 3,4-Methylenedioxyamphetamine/*urine
MH  - Amphetamines/*urine
MH  - Analytic Sample Preparation Methods/*methods
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Humans
MH  - Limit of Detection
MH  - Molecular Structure
MH  - Silicon Dioxide/*chemistry
EDAT- 2010/02/02 06:00
MHDA- 2010/04/01 06:00
CRDT- 2010/02/02 06:00
PHST- 2009/06/22 00:00 [received]
PHST- 2009/12/11 00:00 [revised]
PHST- 2009/12/11 00:00 [accepted]
PHST- 2010/02/02 06:00 [entrez]
PHST- 2010/02/02 06:00 [pubmed]
PHST- 2010/04/01 06:00 [medline]
AID - S0003-2670(09)01666-3 [pii]
AID - 10.1016/j.aca.2009.12.013 [doi]
PST - ppublish
SO  - Anal Chim Acta. 2010 Feb 19;661(1):42-6. doi: 10.1016/j.aca.2009.12.013. Epub 
      2009 Dec 16.