Determination of amphetamine, methamphetamine, 3,4‐methylenedioxyamphetamine, 3,4‐methylenedioxyethylamphetamine, and 3,4‐methylenedioxymethamphetamine in urine by online solid‐phase extraction and ion‐pairing liquid chromatography with detection by electrospray tandem mass spectrometry
Rapid Communications in Mass Spectrometry February 11, 2005 DOI: 10.1002/rcm.1856 via OpenAlex
Summary
AI-generated from the abstractA fully automated method using online solid-phase extraction and ion-pairing liquid chromatography with electrospray tandem mass spectrometry was developed to measure amphetamine, methamphetamine, MDA, MDEA, and MDMA in urine. Recoveries ranged from 85 to 101%. Linear ranges were 10–500 ng/mL for amphetamine and methamphetamine, and dual linear ranges of 5–100 and 100–500 ng/mL for MDA, MDMA, and MDEA. Detection limits were 1–3 ng/mL. Testing on urine samples from drug users showed good agreement with an established GC/MS method.
Study at a glance
| Characteristics | Method development and validation Peer reviewed |
|---|---|
| Population | Urine samples from drug users |
| Keywords | Chromatography Solid phase extraction Detection limit Electrospray Tandem mass spectrometry |
| Citations | 43 |
| Key finding | The automated online SPE-LC/ES-MS/MS method achieved detection limits of 1–3 ng/mL and recoveries of 85–101% for five amphetamine-type drugs in urine. |
Abstract
Abstract A method using an online solid‐phase extraction (SPE) and ion‐pairing liquid chromatography with electrospray tandem mass spectrometry (LC/ES‐MS/MS) was developed for determination of amphetamine (Amp), methamphetamine (mAmp), 3,4‐methylenedioxyamphetamine (MDA), 3,4‐methylenedioxyethylamphetamine (MDEA), and 3,4‐methylenedioxymethamphetamine (MDMA) in urine samples. A SPE cartridge column with both hydrophilic and lipophilic functions was utilized for online extraction. A reversed‐phase C 18 LC column was employed for LC separation and MS/MS was used for detection. Trifluoroacetic acid was added to the mobile phase as an ion‐pairing reagent. This method was fully automated and the extraction and analysis procedures were controlled by a six‐port switch valve. Recoveries ranging from 85–101% were measured. Good linear ranges (10–500 ng/mL) for Amp and mAmp were determined. For MDA, MDMA and MDEA, dual linear ranges were obtained from 5–100 and 100–500 ng/mL, respectively. The detection limit of each analytical compound, based on a signal‐to‐noise ratio of 3, ranged from 1–3 ng/mL. The applicability of this newly developed method was examined by analyzing several urine samples from drug users. Good agreement was obtained between the results from this method and a literature GC/MS method. Copyright © 2005 John Wiley & Sons, Ltd.