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1.
Basic Clin Pharmacol Toxicol ; 125(3): 253-258, 2019 Sep.
Article in English | MEDLINE | ID: mdl-31188528

ABSTRACT

Urine tests are the commonly accepted methods to control abstinence and adherence to treatment of patients who undergo methadone maintenance treatment (MMT). Depending on various national guidelines and accessibility of techniques, only selected psychoactive substances are routinely tested in urine of MMT patients. In general, they belong to the few groups of compounds: THC, cocaine, amphetamines, opiates, PCP and benzodiazepines. It is, however, well known that patients enrolled in such replacement programmes take psychoactive substances that are not routinely detected by the toxicology laboratories, to escape unexpected tests. Here, we report semiquantitative detection of legal highs taken by the MMT patient, using high-pressure liquid chromatography coupled to the flowing atmospheric pressure afterglow ion source (LC-FAPA-MS). To demonstrate effectivity of this technique, the data were confirmed by quantitative analysis using LC-ESI-MS/MS. In the analysed sample of MMT patient, a mixture of psychoactive compounds was found, namely 3-MMC (3-methylmethcathinone), pentedrone and methcathinone and determined at the concentrations of 670; 50 and 0.2 µg/mL, respectively. Such fast analytical technique may be useful for the efficient control of substances taken intentionally by MMT patients.


Subject(s)
Methadone/therapeutic use , Opiate Substitution Treatment/methods , Opioid-Related Disorders/drug therapy , Psychotropic Drugs/urine , Substance Abuse Detection/methods , Chromatography, High Pressure Liquid/methods , Female , Humans , Limit of Detection , Methamphetamine/analogs & derivatives , Methamphetamine/urine , Methylamines/urine , Middle Aged , Opioid-Related Disorders/urine , Patient Compliance , Pentanones/urine , Propiophenones/urine , Tandem Mass Spectrometry/methods
2.
Anal Bioanal Chem ; 409(13): 3393-3405, 2017 May.
Article in English | MEDLINE | ID: mdl-28321502

ABSTRACT

The application of molecularly imprinted polymers (MIPs) as molecular scavengers for ambient plasma ionization mass spectrometry has been reported for the first time. MIPs were synthesized using methacrylic acid as functional monomer; nicotine, propyphenazone, or methylparaben as templates; ethylene glycol dimethacrylate as a cross-linker; and 2,2'-azobisisobutyronitrile as polymerization initiator. To perform ambient plasma ionization experiments, a setup consisting of the heated crucible, a flowing atmospheric-pressure afterglow (FAPA) plasma ion source, and a quadrupole ion trap mass spectrometer has been used. The heated crucible with programmable temperature allows for desorption of the analytes from MIPs structure which results in their direct introduction into the ion stream. Limits of detection, linearity of the proposed analytical procedure, and selectivities have been determined for three analytes: nicotine, propyphenazone, and methylparaben. The analytes used were chosen from various classes of organic compounds to show the feasibility of the analytical procedure. The limits of detections (LODs) were 10 nM, 10, and 0.5 µM for nicotine, propyphenazone, and methylparaben, respectively. In comparison with the measurements performed for the non-imprinted polymers, the values of LODs were improved for at least one order of magnitude due to preconcentration of the sample and reduction of background noise, contributing to signal suppression. The described procedure has shown linearity in a broad range of concentrations. The overall time of single analysis is short and requires ca. 5 min. The developed technique was applied for the determination of nicotine, propyphenazone, and methylparaben in spiked real-life samples, with recovery of 94.6-98.4%. The proposed method is rapid, sensitive, and accurate which provides a new option for the detection of small organic compounds in various samples. Graphical abstract The experimental setup used for analysis.

3.
Anal Bioanal Chem ; 408(3): 815-23, 2016 Jan.
Article in English | MEDLINE | ID: mdl-26563110

ABSTRACT

A thin-layer chromatography-mass spectrometry (TLC-MS) setup for characterization of low molecular weight compounds separated on standard TLC plates has been constructed. This new approach successfully combines TLC separation, laser ablation, and ionization using flowing atmospheric pressure afterglow (FAPA) source. For the laser ablation, a low-priced 445-nm continuous-wave diode laser pointer, with a power of 1 W, was used. The combination of the simple, low-budget laser pointer and the FAPA ion source has made this experimental arrangement broadly available, also for small laboratories. The approach was successfully applied for the characterization of low molecular weight compounds separated on TLC plates, such as a mixture of pyrazole derivatives, alkaloids (nicotine and sparteine), and an extract from a drug tablet consisting of paracetamol, propyphenazone, and caffeine. The laser pointer used was capable of ablating organic compounds without the need of application of any additional substances (matrices, staining, etc.) on the TLC spots. The detection limit of the proposed method was estimated to be 35 ng/cm(2) of a pyrazole derivative.


Subject(s)
Alkaloids/analysis , Chromatography, Thin Layer/methods , Pharmaceutical Preparations/analysis , Pyrazoles/analysis , Atmospheric Pressure , Chromatography, Thin Layer/instrumentation , Laser Therapy
4.
Talanta ; 146: 29-33, 2016.
Article in English | MEDLINE | ID: mdl-26695230

ABSTRACT

Application of a flowing atmospheric-pressure afterglow ion source for mass spectrometry (FAPA-MS) for the analysis of designer drugs is described. In this paper, we present application of FAPA MS for identification of exemplary psychotropic drugs: JWH-122, 4BMC, Pentedrone, 3,4-DNNC and ETH-CAT. We have utilized two approaches for introducing samples into the plasma stream; first in the form of a methanolic aerosol from the nebulizer, and the second based on a release of vapors from the electrically heated crucible by thermal desorption. The analytes were ionized by FAPA and identified in the mass analyzer. The order of release of the compounds depends on their volatility. These methods offer fast and reliable structural information, without pre-separation, and can be an alternative to the Electron Impact, GC/MS, and ESI for fast analysis of designer-, and other psychoactive drugs.


Subject(s)
Atmospheric Pressure , Designer Drugs/analysis , Designer Drugs/chemistry , Mass Spectrometry/methods , Psychotropic Drugs/analysis , Psychotropic Drugs/chemistry , Plasma Gases/chemistry
5.
Analyst ; 140(17): 6138-44, 2015 Sep 07.
Article in English | MEDLINE | ID: mdl-26222687

ABSTRACT

In this paper, a procedure for the preconcentration and transport of mixtures of acids, bases, and drug components to a mass spectrometer using magnetic scavengers is presented. Flowing atmospheric pressure afterglow mass spectrometry (FAPA-MS) was used as an analytical method for identification of the compounds by thermal desorption from the scavengers. The proposed procedure is fast and cheap, and does not involve time-consuming purification steps. The developed methodology can be applied for trapping harmful substances in minute quantities, to transport them to specialized, remotely located laboratories.


Subject(s)
Mass Spectrometry , Benzoic Acid/analysis , Caffeic Acids/analysis , Ferrosoferric Oxide/chemistry , Phthalic Acids/analysis , Polyamines/analysis
6.
Talanta ; 128: 58-62, 2014 Oct.
Article in English | MEDLINE | ID: mdl-25059130

ABSTRACT

The first application of a flowing atmospheric-pressure afterglow ion source for mass spectrometry (FAPA-MS) for the chemical characterization and determination of hexabromocyclododecane (HBCD) is presented. The samples of technical HBCD and expanded polystyrene foam (EPS) containing HBCD as a flame retardant were prepared by dissolving the appropriate solids in dichloromethane. The ionization of HBCD was achieved with a prototype FAPA source. The ions were detected in the negative-ion mode. The ions corresponding to a deprotonated HBCD species (m/z 640.7) as well as chlorine (m/z 676.8), nitrite (m/z 687.8) and nitric (m/z 703.8) adducts were observed in the spectra. The observed isotope pattern is characteristic for a compound containing six bromine atoms. This technique is an effective approach to detect HBCD, which is efficiently ionized in a liquid phase, resulting in high detection efficiency and sensitivity.


Subject(s)
Environmental Pollutants/analysis , Flame Retardants/analysis , Hydrocarbons, Brominated/analysis , Tandem Mass Spectrometry/methods , Atmospheric Pressure , Hydrocarbons, Brominated/chemistry , Ions/chemistry , Methylene Chloride/chemistry , Reproducibility of Results , Tandem Mass Spectrometry/instrumentation
7.
Analyst ; 139(17): 4350-5, 2014 Sep 07.
Article in English | MEDLINE | ID: mdl-25010982

ABSTRACT

The flowing atmospheric pressure afterglow (FAPA) ion source operates in the ambient atmosphere and has been proven to be a promising tool for direct and rapid determination of numerous compounds. Here we linked a FAPA-MS system to an electrochemical flow cell for the identification of drug metabolites generated electrochemically in order to study simulated metabolic pathways. Psychostimulants and their metabolites produced by electrochemistry (EC) were detected on-line by FAPA-MS. The FAPA source has never been used before for an on-line connection with liquid flow, neither for identification of products generated in an electrochemical flow cell. The system was optimized to achieve the highest ionization efficiency by adjusting several parameters, including distances and angles between the ion source and the outlet of the EC system, the high voltage for plasma generation, flow-rates, and EC parameters. Simulated metabolites from tested compounds [methamphetamine (MAF), para-methoxy-N-methylamphetamine (PMMA), dextromethorphan (DXM), and benzydamine (BAM)] were formed in the EC cell at various pH levels. In all cases the main products were oxidized substrates and compounds after N-demethylation. Generation of such products and their thorough on-line identification confirm that the cytochrome P450 - driven metabolism of pharmaceuticals can be efficiently simulated in an electrochemical cell; this approach may serve as a step towards predictive pharmacology using a fast and robust design.


Subject(s)
Anti-Inflammatory Agents/analysis , Benzydamine/analysis , Central Nervous System Stimulants/analysis , Dextromethorphan/analysis , Excitatory Amino Acid Antagonists/analysis , Mass Spectrometry/instrumentation , Methamphetamine/analysis , Anti-Inflammatory Agents/metabolism , Atmospheric Pressure , Benzydamine/metabolism , Central Nervous System Stimulants/metabolism , Cytochrome P-450 Enzyme System/metabolism , Dextromethorphan/metabolism , Electrochemical Techniques/instrumentation , Equipment Design , Excitatory Amino Acid Antagonists/metabolism , Humans , Metabolic Networks and Pathways , Methamphetamine/analogs & derivatives , Methamphetamine/metabolism , Methylation , Oxidation-Reduction
9.
Article in English | MEDLINE | ID: mdl-24428110

ABSTRACT

Computer modeling of the semi-lumped H field-generating multi helical coil, which can be used for generation of H-type discharges at microwave frequencies is presented in this paper. The aim of modeling was to support the design of model plasma source based upon a set of realistic dimensions, which should enable excitation of maximal values of H field at the axis of the discharge tube. As a result, a Microwave-Driven Inductively Coupled Plasma cavity (MICP) has been constructed and its assembly is presented in this paper. The new cavity can be applied in the emission and mass spectroscopy but also can find another applications where maximum H-type coupling is essential.


Subject(s)
Computer-Aided Design , Heating/instrumentation , Microwaves , Models, Theoretical , Plasma Gases/chemical synthesis , Computer Simulation , Equipment Design , Equipment Failure Analysis
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