Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

Analytica Chimica Acta
Akihiro NakamotoAkira Namura

Abstract

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 co...Continue Reading

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Citations

Sep 21, 2010·Analytical and Bioanalytical Chemistry·Li XuYu-Qi Feng
Feb 6, 2013·Analytical and Bioanalytical Chemistry·Dustin R Bunch, Sihe Wang
Jun 22, 2013·Journal of Pharmaceutical and Biomedical Analysis·Tarang NemaPaul C Ho
Sep 9, 2011·Bioanalysis·Victoria SamanidouKonstantinos Rentifis
Nov 10, 2010·Biomedical Chromatography : BMC·Stacy D Brown, Tyler C Melton
Sep 5, 2015·Bioanalysis·Akira Namera, Takashi Saito
Jul 30, 2015·Journal of Pharmaceutical and Biomedical Analysis·Erina TamashimaHitoshi Nohta
Dec 13, 2018·Bioanalysis·Shahram SeidiReza Alizadeh
Feb 13, 2020·Mass Spectrometry Reviews·Scott A BordenPierangela Palma
Mar 12, 2011·Journal of Separation Science·Akira NameraShota Miyazaki
Dec 2, 2020·Asian-Australasian Journal of Animal Sciences·Chaoyan FengChunbao Li

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