scholarly journals Rapid Targeted Method of Detecting Abused Piperazine Designer Drugs

2021 ◽  
Vol 10 (24) ◽  
pp. 5813
Author(s):  
Anna Welz ◽  
Marcin Koba ◽  
Piotr Kośliński ◽  
Joanna Siódmiak
Keyword(s):  
Analytical Approach ◽  
Detection Method ◽  
Designer Drugs ◽  
Internal Standards ◽  
Piperazine Derivatives ◽  
Qualitative Evidence ◽  
Laboratory Confirmation ◽  
Target Analytes ◽  
Product Ions ◽  
Recreational Use

Piperazine derivatives belong to the popular psychostimulating compounds from the group of designer drugs. They are an alternative to illegal drugs such as ecstasy and amphetamines. They are being searched by consumers for recreational use due to their stimulating and hallucinogenic effects. Many NPS-related poisonings and deaths have been reported where piperazines have been found. However, a major problem is the potential lack of laboratory confirmation of the involvement of piperazine derivatives in the occurrence of poisoning. Although many methods have been published, piperazine derivatives are not always included in a routine analytical approach or targeted toxicological analysis. There is an increasing need to provide qualitative evidence for the presence of piperazine derivatives and to ensure reproducible quantification. This article describes a new rapid method of detecting piperazine derivatives in biological material, using LC-MS. All target analytes were separated in a 15 min run time and identified based on the precursor ion, at least two product ions, and the retention time. Stable isotopically labeled (SIL) internal standards: BZP-D7, mCPP-D8 and TFMPP-D4 were used for analysis, obtaining the highest level of confidence in the results. The proposed detection method provides the analytical confirmation of poisoning with piperazine designer drugs.

Methylenedioxymethamphetamine (MDMA): a.k.a. Ecstasy

2020 ◽  
Author(s):  
Jerrold Winter
Keyword(s):  
Therapeutic Potential ◽  
Illegal Drug ◽  
The Other ◽  
Designer Drugs ◽  
Pharmacological Effects ◽  
Other Hand ◽  
Gamma Hydroxybutyrate ◽  
Amphetamine Derivatives ◽  
Recreational Use ◽  
Vanderbilt University

As these words are written, the chemical we will call MDMA is a Schedule I drug. This means that MDMA (a) has no currently accepted medical use, (b) no currently accepted safety even under medical supervision, and (c) has a high potential for abuse. On the other hand, there are those who see great therapeutic potential in MDMA, and the Food and Drug Administration (FDA) has designated MDMA- assisted psychotherapy as a breakthrough therapy. We can foresee the day when it will be available by prescription. There is no doubt as to the chemical identity of MDMA, and much is known of its pharmacological effects in humans and in animals. The recreational drug commonly known as Ecstasy is more complicated. As is true for any illegal drug used by millions of people, demand for the drug has been met by persons not noted for their high ethical or manufacturing standards. Simply stated, short of chemical analysis, one can never be sure what street-bought Ecstasy is. For example, investigators at Vanderbilt University determined the contents of 1,214 tablets sold as Ecstasy. Only 39% contained only MDMA, while fully 46% were “substances other than MDMA.” Mixtures of MDMA and other drugs comprised the remaining 15%. On the other hand, sometimes in some places over the past several decades, nearly pure MDMA has been available on the illicit market. Nonetheless, a buyer of Ecstasy may ingest, rather than MDMA, drugs such as ketamine, gamma-hydroxybutyrate (GHB), cathinone, ephedrine, caffeine, or any one of the so-called designer drugs, many of which are amphetamine derivatives. A consequence of this pharmacological chaos is that many of the hazards associated with the use of Ecstasy have been uncritically attributed to MDMA. This fact has been a boon for those who would continue the Schedule I status of MDMA and a bane for those who would explore its therapeutic potential. However, in contrast with recreational use where purity of the drug is uncertain, MDMA in clinical trials is FDA approved and of known composition.

scholarly journals Analysis for Alpha-Pyrrolidinovalerophenone and Its 2-Oxo-PVP Metabolite in Plasma by Liquid Chromatography–Tandem Mass Spectrometry

2019 ◽  
Author(s):  
David M Andrenyak ◽  
David E Moody ◽  
Jonathan M Crites ◽  
Michael H Baumann
Keyword(s):  
Room Temperature ◽  
Rat Plasma ◽  
Sample Volume ◽  
Internal Standards ◽  
Accuracy And Precision ◽  
Assay Performance ◽  
Liquid Chromatography Tandem Mass ◽  
Assay Precision ◽  
Recreational Use ◽  
Positive Ion

Abstract Alpha-pyrrolidinovalerophenone (alpha-PVP), a novel psychoactive substance, has widespread recreational use. This with interest in its pharmacological effects creates a need for methods that measure alpha-PVP concentrations. We therefore developed a LC-MS/MS method that can quantitate alpha-PVP and 2-oxo-PVP in rat plasma using a 0.1-mL sample volume. Addition of internal standards (2.5 ng/mL alpha-PVP-d8/2-oxo-PVP-d6) was followed by liquid–liquid extraction with 1-chlorobutane:acetonitrile (4:1), evaporation and reconstitution with 0.1% formic acid. Extracts were analyzed by LC-MS/MS using an Agilent 1100 HPLC and a Thermo Scientific TSQ Quantum Access MS/MS, with a YMC ODS-AQ, 50 mm × 2 mm, 3 μm column. The mobile phase was 0.1% formic acid:acetonitrile gradient at a 0.2-mL/minute flow rate with positive ion electrospray. SRM was used for the analysis with transitions: alpha-PVP, 232 → 91; alpha-PVP-d8, 240 → 91; 2-oxo-PVP, 246 → 91; 2-oxo-PVP-d6, 252 → 91. Alpha-PVP and 2-oxo-PVP eluted at 6.4 and 8.9 min. Calibrators range from 0.25 to 500 ng/mL. Accuracy and precision evaluated quality control samples prepared at 0.75, 10 and 400 ng/mL. The intra-assay evaluation also included the 0.25-ng/mL LOQs prepared in six different blank plasma sources. The intra-assay accuracy ranged from 88.9 to 117.8% of the target, and the intra-assay precision ranged from 0.9 to 16.0%. The inter-assay accuracy ranged from 98.7 to 110.7% of the target, and the inter-assay precision ranged from 4.5 to 12.0%. Extraction recovery was at least 52% for alpha-PVP and 67% for 2-oxo-PVP. Ionization recoveries were at least 64% for alpha-PVP and 82% for 2-oxo-PVP. These losses did not adversely affect assay performance. Alpha-PVP and 2-oxo-PVP controls were stable at room temperature for up to 24 h and frozen for at least 36 days. Alpha-PVP and 2-oxo-PVP were also stable in processed samples (extracts) stored at room temperature for at least 24 days. The procedure was used to analyze rat plasma samples from a pharmacokinetic study.

Recreational use of carfentanil – a case report with laboratory confirmation

2017 ◽  
Vol 56 (2) ◽  
pp. 151-152 ◽  
Author(s):  
Sabine Müller ◽  
Susanne Nussbaumer ◽  
Gabriel Plitzko ◽  
Roger Ludwig ◽  
Wolfgang Weinmann ◽  
...  
Keyword(s):  
Case Report ◽  
Laboratory Confirmation ◽  
Recreational Use

scholarly journals Electrosynthesized Poly(o-aminophenol) Films as Biomimetic Coatings for Dopamine Detection on Pt Substrates

Chemosensors ◽  
2021 ◽  
Vol 9 (10) ◽  
pp. 280
Author(s):  
Rosanna Ciriello ◽  
Martina Graziano ◽  
Giuliana Bianco ◽  
Antonio Guerrieri
Keyword(s):  
Molecularly Imprinted Polymers ◽  
Electrochemical Sensors ◽  
Detection Method ◽  
Limit Of Detection ◽  
Oxidation Products ◽  
Experimental Conditions ◽  
Easy Method ◽  
Dopamine Detection ◽  
Target Analytes ◽  
Mip Sensor

Dopamine (DA) is a neurotransmitter, and its levels in the human body are associated with serious diseases. The need for a suitable detection method in medical practice has encouraged the development of electrochemical sensors that take advantage of DA electroactivity. Molecularly imprinted polymers (MIPs) are biomimetic materials able to selectively recognize target analytes. A novel MIP sensor for DA is proposed here based on a thin film of poly(o-aminophenol) electrosynthesized on bare Pt. A fast and easy method for executing the procedure for MIP deposition has been developed based on mild experimental conditions that are able to prevent electrode fouling from DA oxidation products. The MIP exhibited a limit of detection of 0.65 μM, and appreciable reproducibility and stability. The high recognition capability of poly(o-aminophenol) towards DA allowed for the achievement of notable selectivity: ascorbic acid, uric acid, serotonin, and tyramine did not interfere with DA detection, even at higher concentrations. The proposed sensor was successfully applied for DA detection in urine samples, showing good recovery.

Metabolism of designer drugs. Piperazine derivatives

2015 ◽  
Vol 58 (4) ◽  
pp. 49
Author(s):  
A. B. Melent’ev ◽  
S. S. Kataev
Keyword(s):  
Designer Drugs ◽  
Piperazine Derivatives

scholarly journals Out with the old, in with the new? Case reports of the clinical features and acute management of two novel designer drugs

2012 ◽  
Vol 11 (3) ◽  
pp. 157-160
Author(s):  
E J Hamilton ◽  
◽  
Gary Peter Misselbrook ◽  
Keyword(s):  
Clinical Features ◽  
Case Reports ◽  
Designer Drugs ◽  
Acute Management ◽  
Medical Journals ◽  
Recreational Use

Methoxydine (4-MeO-PCP) and Methoxetamine (3-MeO-2-Oxo-PCE) are both commercially produced designer drugs with structural and biochemical similarities to phencyclidine (PCP). Although phencyclidine toxicity is well documented, its recreational use in present times is rare. With the advent of new designer drugs being available widely through internet sites, Acute Physicians should be aware of the clinical features and management of these potential toxins. We present a case of methoxydine ingestion (which to our knowledge has not been previously documented in any medical journals) and a case of methoxetamine ingestion, and discuss their history, contrasting clinical features and acute management.

scholarly journals Synthesis and characterization of Zr- and Hf-doped nano-TiO 2 as internal standards for analytical quantification of nanomaterials in complex matrices

2018 ◽  
Vol 5 (6) ◽  
pp. 171884 ◽  
Author(s):  
Laura-Jayne A. Ellis ◽  
Anastasios G. Papadiamantis ◽  
Stefan Weigel ◽  
Eugenia Valsami-Jones
Keyword(s):  
Electron Microscopy ◽  
Inductively Coupled Plasma ◽  
Optical Emission ◽  
Complex Matrices ◽  
Internal Standards ◽  
X Ray ◽  
Analytical Process ◽  
Inductively Coupled ◽  
Target Analytes ◽  
Analytical Quantification

The reliable quantification of nanomaterials (NMs) in complex matrices such as food, cosmetics and biological and environmental compartments can be challenging due to interactions with matrix components and analytical equipment (vials and tubing). The resulting losses along the analytical process (sampling, extraction, clean-up, separation and detection) hamper the quantification of the target NMs in these matrices as well as the compatibility of results and meaningful interpretations in safety assessments. These issues can be overcome by the addition of known amounts of internal/recovery standards to the sample prior to analysis. These standards need to replicate the behaviour of target analytes in the analytical process, which is mainly defined by the surface properties. Moreover, they need to carry a tag that can be quantified independently of the target analyte. As inductively coupled plasma mass spectrometry is used for the identification and quantification of NMs, doping with isotopes, target analytes or with chemically related rare elements is a promising approach. We present the synthesis of a library of TiO 2 NMs doped with hafnium (Hf) and zirconium (Zr) (both low in environmental abundance). Zirconia NMs doped with Hf were also synthesized to complement the library. NMs were synthesized with morphological and size properties similar to commercially available TiO 2 . Characterization included: transmission electron microscopy coupled with energy-dispersive X-ray spectroscopy, X-ray diffraction spectroscopy, Brunauer–Emmett–Teller total specific surface area analysis, cryofixation scanning electron microscopy, inductively coupled plasma optical emission spectroscopy and UV–visible spectrometry. The Ti : Hf and Ti : Zr ratios were verified and calculated using Rietveld refinement. The labelled NMs can serve as internal standards to track the extraction efficiency from complex matrices, and increase method robustness and traceability of characterization/quantification.

scholarly journals Novel Fast Chromatography-Tandem Mass Spectrometric Quantitative Approach for the Determination of Plant-Extracted Phytosterols and Tocopherols

Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1402
Author(s):  
George Gachumi ◽  
Alice Demelenne ◽  
Asmita Poudel ◽  
Zafer Dallal Bashi ◽  
Anas El-Aneed
Keyword(s):  
Quantitative Analysis ◽  
Mass Spectrometric ◽  
Deodorizer Distillate ◽  
Tandem Mass ◽  
Internal Standards ◽  
Target Analytes ◽  
Tandem Mass Spectrometric ◽  
Pharmaceutical Industries ◽  
Accurate Quantification

Phytosterols and tocopherols are commonly used in food and pharmaceutical industries for their health benefits. Current analysis methods rely on conventional liquid chromatography, using an analytical column, which can be tedious and time consuming. However, simple, and fast analytical methods can facilitate their qualitative and quantitative analysis. In this study, a fast chromatography-tandem mass spectrometric (FC-MS/MS) method was developed and validated for the quantitative analysis of phytosterols and tocopherols. Omitting chromatography by employing flow injection analysis—mass spectrometry (FIA-MS) failed in the quantification of target analytes due to analyte-to-analyte interferences from phytosterols. These interferences arise from their ambiguous MS fingerprints that would lead to false identification and inaccurate quantification. Therefore, a C18 guard column with a 1.9 µm particle size was employed for FC-MS/MS under isocratic elution using acetonitrile/methanol (99:1 v/v) at a flow rate of 600 µL/min. Analyte-to-analyte interferences were identified and eliminated. The false peaks could then be easily identified due to chromatographic separation. In addition, two internal standards were evaluated, namely cholestanol and deuterated cholesterol. Both internal standards contributed to the observed analyte-to-analyte interferences; however, adequate shift in the retention time for deuterated cholesterol eliminated its interferences and allowed for an accurate quantification. The method is fast (1.3 min) compared to published methods and can distinguish false peaks observed in FIA-MS. Seven analytes were quantified simultaneously, namely brassicasterol, campesterol, stigmasterol, β-sitosterol, α-tocopherol, δ-tocopherol, and γ-tocopherol. The method was successfully applied in the quantitative analysis of phytosterols and tocopherols present in the unsaponifiable matter of canola oil deodorizer distillate (CODD). β-sitosterol and γ-tocopherol were the most abundant phytosterols and tocopherols, respectively.

scholarly journals GC-MS/MS method for simultaneous determination of ester forms of 3-MCPD and 2-MCPD in infant formula

2020 ◽  
Vol 3 (2) ◽  
pp. 133-144
Author(s):  
Chi Le Dinh ◽  
Thuong Nguyen Nhu ◽  
Tu Vu Ngoc ◽  
Hong Hao Le Thi ◽  
Son Tran Cao ◽  
...  
Keyword(s):  
Sulfuric Acid ◽  
Infant Formula ◽  
Flow Rate ◽  
Mobile Phase ◽  
Capillary Column ◽  
Phenylboronic Acid ◽  
Tandem Mass ◽  
Internal Standards ◽  
Product Ions

A sensitive GC-MS/MS method has been developed and validated for determining ester forms of 3-MCPD and 2-MCPD in infant formula, using 3-MCPD-d5 and 2-MCPD-d5 as internal standards, respectively. The esters of MCPDs were extracted from infant formula powder with mixture of ethanol/n-hexane/diethyl ether (1/1/1, v/v/v), then treated with sulfuric acid to release free MCPDs. Free MCPDs and internal standards were derivatized with phenylboronic acid and the corresponding derivatives were used for GC-MS/MS analysis. The chromatographic separation was performed in a DB-5MS capillary column using helium as mobile phase at flow rate of 1 mL/min. Tandem mass spectroscopic detection of each analyte was done in MRM mode by monitoring one precursor ion and two product ions. Validation results confirmed the suitability of the developed method for intended application. Application of the method in samples collected from different provinces in Vietnam detected esterified 3-MCPD in 38.9% of samples, esterified 2-MCPD in 34.7% of samples.

scholarly journals Recent Progress on Sensing Application of Metal Nanoarchitectures Enhanced Fluorescence

2021 ◽  
Author(s):  
Meiling Wang
Keyword(s):  
Analytical Method ◽  
Analytical Approach ◽  
Recent Progress ◽  
High Sensitivity ◽  
Enhanced Fluorescence ◽  
Non Invasive ◽  
Target Analytes ◽  
Sensing Application ◽  
Invasive Measurement

Fluorescence analytical method, as a real time and in situ analytical approach to target analytes, can offer advantages of high sensitivity/selectivity, great versatility, non-invasive measurement and easy to transmit over...

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