Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection
| Autor: | Akihiro Nakamoto, Shota Miyazaki, Manami Nishida, Takeshi Saito, Masataka Nagao, Akira Namura, Izumi Kishiyama, Katsunori Murakami |
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| Rok vydání: | 2010 |
| Předmět: |
Detection limit
Chromatography Molecular Structure Elution Amphetamines Extraction (chemistry) Analytic Sample Preparation Methods Urine Silicon Dioxide Mass spectrometry Biochemistry Gas Chromatography-Mass Spectrometry Analytical Chemistry chemistry.chemical_compound chemistry Limit of Detection Spin column-based nucleic acid purification Humans Environmental Chemistry Gas chromatography–mass spectrometry Derivatization 3 4-Methylenedioxyamphetamine Spectroscopy |
| Zdroj: | Analytica Chimica Acta. 661:42-46 |
| ISSN: | 0003-2670 |
| DOI: | 10.1016/j.aca.2009.12.013 |
| Popis: | 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 correlationor = 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 ratioor = 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. |
| Databáze: | OpenAIRE |
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