Two-side slug-flow microextraction coupled with ion mobility spectrometry for fast quantification of amphetamine and methamphetamine in human urine
In this study, first time a novel slug-flow microextraction (SFME) procedure named two-side SFME was developed and followed by ion mobility spectrometry equipped with corona discharge source (CD-IMS) for quantification of two abused drugs (amphetamine (AM) and methamphetamine (ME)) in urine samples. Regarding technique workflow, the organic extraction solvent (10 μL) was sandwiched between two portions of aqueous sample solution (the volume of each portion of sample solution was 5 μL) into a disposable glass capillary tube. The extraction of analytes was performed via the slug flows induced by the movements of the three liquids, which was conducted by tilting the glass capillary tube for several cycles. Finally, the extraction solvent was collected by a microsyringe and then injected (5 μL) into the CD-IMS. The effects of the effective parameters, including type of extraction solvent, number of tilting the glass capillary tube, and concentration of salt in sample solution were investigated. Under the optimized extraction condition (organic solvent: toluene; number of tilting the glass capillary tube: 10 times; concentration of salt: 5% (w/v)), the proposed two-side SFME/CD-IMS provided good linearity with coefficients of determination ≥0.993 over a concentration range of 25.0–2000.0 ng mL−1. Accordingly, acceptable limits of detection (S/N = 3) were 10.0 and 2.5 ng mL−1 for AM and ME, respectively. Furthermore, acceptable recoveries were ≥ 81.5, and ≥ 88.0% for AM and ME in a human urine sample, respectively, while repeatability and reproducibility ranged from 6.7 to 14.7% (n = 3).
- Research Article
12
- 10.1016/j.aca.2018.03.057
- Apr 18, 2018
- Analytica Chimica Acta
Rapid and accurate quantification of amphetamine and methamphetamine in human urine by antibody decorated magnetite nanoparticles coupled with matrix-assisted laser desorption ionization time-of-flight mass spectrometer analysis
- Research Article
58
- 10.1016/j.chroma.2009.05.074
- Jun 2, 2009
- Journal of Chromatography A
Solvent-bar microextraction—Using a silica monolith as the extractant phase holder
- Research Article
89
- 10.1016/0925-4005(93)85358-h
- May 1, 1993
- Sensors and Actuators B: Chemical
Piezoelectric crystal immunosensor for sensitive detection of methamphetamine (stimulant drug) in human urine
- Research Article
88
- 10.1016/j.aca.2005.09.063
- Oct 28, 2005
- Analytica Chimica Acta
Novel fiber coated with β-cyclodextrin derivatives used for headspace solid-phase microextraction of ephedrine and methamphetamine in human urine
- Research Article
76
- 10.1016/j.talanta.2019.02.027
- Mar 5, 2019
- Talanta
Ultra-trace detection of methamphetamine in biological samples using FFT-square wave voltammetry and nano-sized imprinted polymer/MWCNTs -modified electrode
- Research Article
64
- 10.1016/j.jpba.2005.06.023
- Aug 1, 2005
- Journal of Pharmaceutical and Biomedical Analysis
Liquid-phase microextraction combined with high-performance liquid chromatography for the determination of local anaesthetics in human urine
- Research Article
4
- 10.30492/ijcce.2020.128885.4177
- Dec 5, 2020
- Iranian Journal of Chemistry & Chemical Engineering-international English Edition
A highly sensitive, simple and speed technique was employed for the determination of brilliant green in fish (Sphyraena jello) and seawater samples by visible spectrophotometry after its extraction and enrichment with chitosan- zinc oxide nanoparticle coupled with dispersive liquid- liquid microextraction. Ultra-trace concentrations of brilliant green were dispersed to organic phase in DLLME method after adding of dispersive solvent and chitosan- zinc oxide nanoparticles. The experimental factors such as amount of chitosan- zinc oxide nanoparticles, concentration of Triton X- 114, type of volume of extraction and dispersive solvents, extraction time, rate and time of centrifugation, volume of sample and pH were investigated to order to enhance of the extraction efficiency. Under optimum extraction condition, volume of chloroform (as extraction solvent) and methanol (as dispersive solvent) were 100.0 µL and 550.0 µL, respectively; amount of chitosan- zinc oxide nanoparticles was 15.0 mg; time of extraction was 4.0 min; rate and time of centrifugation were 3000.0 rpm and 8.0 min, respectively, volume of sample was 8.0 mL, and pH of sample solution was 4.0. After optimizing of the microextraction conditions and instrumental factors, an enrichment factor of 169.0 was achieved. The analytical curve )absorbance vs. concentration( was linear over the range 1.0-200.0 µg/L of brilliant green. The limit of detection and relative standard deviation were 0.3 µg/L and < 6.1 %, respectively. The protocol was successfully employed to the determination of brilliant green in seawater of Chabahar Bay and fish (Sphyraena jello) samples.
- Research Article
33
- 10.1520/jfs2003233
- Jan 1, 2004
- Journal of Forensic Sciences
The purpose of this study was to evaluate the ability of two amphetamine class screening reagents to exclude ephedrine (EPH), pseudoephedrine (PSEPH), and phenylpropanolamine (PPA) from falsely producing positive immunoassay screening results. The study also sought to characterize the prevalence and concentration distributions of EPH, PSEPH, and PPA in samples that produced positive amphetamine screening results. Approximately 27,400 randomly collected human urine samples from Navy and Marine Corps members were simultaneously screened for amphetamines using the DRI and Abuscreen online immunoassays at a cutoff concentration of 500 ng/mL. All samples that screened positive were confirmed for amphetamine (AMP), methamphetamine (MTH), 3,4-Methylenedioxyamphetamine (MDA), 3,4-Methylenedioxymethamphetamine (MDMA), EPH, PSEPH, and PPA by gas chromatography/mass spectrometry (GC/MS). The DRI AMP immunoassay identified 1,104 presumptive amphetamine positive samples, of which only 1.99% confirmed positive for the presence of AMP, MTH, MDA, or MDMA. In contrast, the online AMP reagent identified 317 presumptive amphetamine positives with a confirmation rate for AMP, MTH, MDA, or MDMA of 7.94%. The presence of EPH, PSEPH, or PPA was confirmed in 833 of the 1,104 samples that failed to confirm positive for AMP, MTH, MDA, or MDMA; all of the 833 samples contained PSEPH. When compared to the entire screened sample set, PSEPH was present in approximately 3%, EPH in 0.9%, and PPA in 0.8% of the samples. The results indicate that cross reactivities for EPH, PSEPH, and PPA are greater than reported by the manufacturer of these reagents. The distribution of concentrations indicates that very large concentrations of EPH, PSEPH, and PPA are common.
- Research Article
224
- 10.1016/j.aca.2008.02.057
- Mar 5, 2008
- Analytica Chimica Acta
Cold-induced aggregation microextraction: A novel sample preparation technique based on ionic liquids
- Research Article
5
- 10.1007/s12127-013-0137-1
- May 30, 2013
- International Journal for Ion Mobility Spectrometry
The major reactant ion in conventional ion mobility spectrometry (IMS) is the hydronium ion, H3O+ which is produced in the usual ionization sources such as corona discharge or radioactive sources. Using the hydronium reactant ion, mostly the analytes with proton affinity higher than that of water are ionized. A broader range of compounds can be detected by IMS if other alternative ionization channels, such as charge transfer from NO+, are employed. In this work we introduce a simple and novel method for producing NO+ as the major reactant ion in IMS. This was achieved by adding neutral NO to the corona discharge ionization source. The neutral NO was prepared via an additional discharge in an air stream, flowing into the corona discharge source. A curtain plate was mounted in front of the corona discharge to prevent the influence of the analyte on the production of NO+. Using this technique, the reactant ion could easily and quickly switch between the H3O+ and NO+. The performance of the new source was evaluated by recording ion mobility spectra of test compounds with both H3O+ and NO+ reactant ions.
- Research Article
4
- 10.1016/j.jmsacl.2025.07.001
- Aug 1, 2025
- Journal of mass spectrometry and advances in the clinical lab
Urine methamphetamine-to-amphetamine ratio by LC-MS/MS to differentiate methamphetamine use from pharmaceutical impurity in patients prescribed amphetamine.
- Research Article
185
- 10.1007/s00213-002-1288-7
- Dec 19, 2002
- Psychopharmacology
Methamphetamine (METH) and amphetamine (AMPH) are both abused psychostimulants. Although METH is generally accepted to be more addictive and potent than its analogue AMPH, there are no known neurobiological differences in action between the two drugs that may account for such differences. METH and AMPH were compared to determine potential mechanisms for such differences between the two drugs in order to provide new targets for the treatment of METH addiction. Using in vivo microdialysis on rats, dopamine (DA), DA metabolites, and glutamate (GLU) release in the nucleus accumbens (NAC) and prefrontal cortex (PFC) were measured after administration of 2 mg/kg, IP, of METH or AMPH. Based on the neurochemical differences between METH and AMPH, a locomotor activity study was designed to assess differences in locomotor activation for a range of doses (1-4 mg/kg, IP) of METH and AMPH and after pretreatment with intra-accumbens GLU antagonists. METH and AMPH raised NAC DA levels to a similar degree. In the PFC, both METH and AMPH raised DA levels, but METH was less effective than AMPH. In the NAC, AMPH raised GLU levels but METH did not. In the PFC, METH raised GLU levels but AMPH did not. The locomotor activity dose response curve for METH had a lower peak than that of AMPH. This difference was blocked by pretreatment with either the GLU NMDA antagonist AP5 or the GLU AMPA antagonist DNQX locally in the NAC. This study reveals several previously unknown neurochemical and behavioral differences between METH and AMPH. Based on these results, it is suggested that new pharmacotherapeutic agents that produce augmentations of NAC GLU or PFC DA activity, or perhaps inhibition of PFC GLU activity, may someday be useful for the treatment of METH addiction.
- Research Article
9
- 10.1007/s11419-006-0009-z
- Aug 1, 2006
- Forensic Toxicology
Monolithic silica capillary column extraction of methamphetamine and amphetamine in urine coupled with thin-layer chromatographic detection
- Research Article
5
- 10.1021/ac062229o
- Apr 24, 2007
- Analytical Chemistry
Stereoisomeric identification of norephedrine (NE) derived from methamphetamine (MA) or amphetamine (AM) was investigated by SIM-GC/MS assay using the urine of 33 MA abusers and 1 AM abuser. The assay simultaneously identified TFA-derivatized MA and AM metabolites, including AM, p-hydroxyl-MA (p-HMA), and p-hydroxyl-AM (p-HAM). The analysis lasted approximately 43 min, with a signal-to-noise ratio of >or=3 and a detection limit of 50 ng/mL. Among 12 urine samples from different subjects, only the S (+) form of MA and its metabolites (AM, p-HMA, p-HAM) was detected, however, a (1R,2S)-(-)-NE stereoisomer was also identified. Among the urine samples of two subjects, only the R (-) form of MA and its metabolites (AM, p-HMA, p-HAM) was detected, while NE was not detected. Following urinalysis of urine obtained from 19 MA abusers and 1 AM abuser, only the (1R,2S)-(-)-NE stereoisomer was identified, while unmetabolized MA, AM, and their metabolites (p-HMA, p-HAM), showed stereoselective metabolism. Although (1R,2S)-(-)-ephedrine (EP) alone was found in the urine of 1 (S)-(+)-MA user and 1 (S)-(+)- and (R)-(-)-MA user among 33 MA users, it was not present in the urine of the remaining 31 subjects. Therefore, (1R,2S)-(-)-NE was likely not of (1R,2S)-(-)-EP origin and was most likely from (S)-(+)-AM of the MA metabolite. The production ratio of (1R,2S)-(-)-NE to (S)-(+)-AM ranged from 0.01 to 0.25 in MA abusers and was 0.12 in AM abusers.
- Research Article
47
- 10.1016/j.talanta.2014.01.005
- Jan 15, 2014
- Talanta
Miniaturized salting-out liquid–liquid extraction in a coupled-syringe system combined with HPLC–UV for extraction and determination of sulfanilamide