Stability of Synthetic Piperazines in Human Whole Blood.

Abstract:

:While circumventing legislative controls, synthetic piperazines are encountered as "legal" alternatives to ecstasy. Unforeseeable challenges may delay quantitative analysis of these compounds in biological fluids. Enzymatic reactions, matrix interferences and limited knowledge of analyte stability further complicate interpretation of calculated concentrations. The objective of this study was to investigate the stability of synthetic piperazines in human blood under various storage conditions over time. All samples were prepared by spiking certified reference standards (Cayman Chemical, MI, U.S.A.) of eight synthetic piperazine into certified drug-free human whole blood (UTAK Laboratories, Inc., CA, U.S.A.) independently at 1000 ng/mL as well as mixtures containing all tested piperazines in this study. Samples were stored at room temperature (~20°C), 4°C and -20°C for 1, 3, 6, 9 and 12 months in dark sealed containers. Solid phase extraction (SPE) was performed using mixed-mode copolymeric cartridges (Clean Screen®, UCT Inc., PA, U.S.A.). Analytes were assessed on their degrees of degradation using a Shimadzu Ultra-Fast Liquid Chromatograph with SCIEX 4000 Q-Trap Electrospray Ionization Tandem Mass Spectrometer (UFLC-ESI-MS/MS) in positive ionization mode. Of the two categories, benzyl piperazines were more stable than phenyl piperazines under all storage conditions, in which 1-(4-methylbenzyl)-piperazine (MBZP) had more than 70% (769-1,047 ng/mL) remaining after 12 months. 1-(4-methoxyphenyl)-piperazine (MeOPP) was not detected under room and refrigerated temperatures after 6 months and was the least stable. Matrix interferences and drug-drug interaction were observed. Storing samples at room temperature should be avoided due to detrimental impacts on stability of piperazine compounds. For backlog situations, case samples suspected to contain synthetic piperazines should be kept frozen or refrigerated even for time periods as short as 30 days for optimal result. Phenyl piperazines stored for more than 6 months showed analyte degradation and loss of parent compounds after extended storage regardless of storage conditions.

journal_name

J Anal Toxicol

authors

Lau T,LeBlanc R,Botch-Jones S

doi

10.1093/jat/bkx090

subject

Has Abstract

pub_date

2018-03-01 00:00:00

pages

88-98

issue

2

eissn

0146-4760

issn

1945-2403

pii

4656137

journal_volume

42

pub_type

杂志文章
  • fMRI: a new tool for the in vivo localization of drug actions in the brain.

    abstract::Functional magnetic resonance imaging (fMRI), a still-emerging, non-invasive neuroimaging tool, has been applied to a wide range of questions in sensory, motor control, and cognitive psychology. Only more recently has it been applied to understand the sites and mechanisms of action of pharmacological agents within the...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章,评审

    doi:10.1093/jat/25.5.419

    authors: Stein EA

    更新日期:2001-07-01 00:00:00

  • Multiple Drug-Toxicity Involving Novel Psychoactive Substances, 3-Fluorophenmetrazine and U-47700.

    abstract::3-Fluorophenmetrazine (3-FPM) is a stimulant-like novel psychoactive substance (NPS) and fluorinated analog of phenmetrazine that has recently appeared on the recreational drug market, with limited published information. Likewise, the synthetic opioid U-47700 has gained popularity among recreational drug users and is ...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/bkx060

    authors: Ellefsen KN,Taylor EA,Simmons P,Willoughby V,Hall BJ

    更新日期:2017-11-01 00:00:00

  • Measurement of lysergic acid diethylamide (LSD) in human plasma by gas chromatography/negative ion chemical ionization mass spectrometry.

    abstract::A previously reported procedure for quantification of LSD in urine was modified to permit measurement of the drug in plasma. After addition of deuterium-labelled LSD, the plasma is extracted and the extract is treated with trifluoroacetylimidazole to convert the LSD to its N-trifluoroacetyl derivative. The derivatized...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/14.3.189

    authors: Papac DI,Foltz RL

    更新日期:1990-05-01 00:00:00

  • Bone surface and whole bone as biomarkers for acute fluoride exposure.

    abstract::This study compares fluoride concentrations ([F]) in surface and whole bone for up to 27 days following an acute oral dose of F. Four groups of rats received single oral F dose (50 mg/kg body weight), and the control group received deionized water (n = 10/group). Groups were euthanized at 1, 3, 9, or 27 days after F a...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/29.8.810

    authors: Buzalaf MA,Caroselli EE,de Carvalho JG,de Oliveira RC,da Silva Cardoso VE,Whitford GM

    更新日期:2005-11-01 00:00:00

  • Validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair.

    abstract::A liquid chromatography-tandem mass spectrometry method was developed for the simultaneous quantification of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair. Drugs were extracted from all matrices by liquid-liquid extraction with 1-chlorobutane. Chromatography was achieved using a...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/29.7.616

    authors: Laloup M,Ramirez Fernandez Mdel M,De Boeck G,Wood M,Maes V,Samyn N

    更新日期:2005-10-01 00:00:00

  • Quantitation of diethylene glycol and its metabolites by gas chromatography mass spectrometry or ion chromatography mass spectrometry in rat and human biological samples.

    abstract::The misuse of the commonly used chemical diethylene glycol (DEG) has lead to many poisonings worldwide. Methods were developed for analysis of DEG and its potential metabolites; ethylene glycol, glycolic acid, oxalic acid, diglycolic acid and hydroxyethoxy acetic acid in human urine, serum and cerebrospinal fluid samp...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/bku018

    authors: Perala AW,Filary MJ,Bartels MJ,McMartin KE

    更新日期:2014-05-01 00:00:00

  • A thin layer chromatographic method for high volume screening of urine for methylphenidate abuse.

    abstract::A thin layer chromatographic (TLC) method for the high volume screening of urine for methylphenidate (Ritalin) abuse is presented. The method utilizes charcoal extraction of ritalinic acid from urine and a simple test-tube methylation step for the conversion of the ritalinic acid to methylphenidate. The methylphenidat...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/10.3.116

    authors: Manno BR,Manno JE,Dempsey CA

    更新日期:1986-05-01 00:00:00

  • Quantitative endogenous formate analysis in plasma using headspace gas chromatography without a headspace analyzer.

    abstract::The objective was to develop a simple routine method for quantitative measurement of endogenous formic acid in plasma and whole blood using headspace gas chromatography-flame ionization detection. (GC-FID). Two-hundred microliters of sample was placed in a 1-mL glass vial. Fifty microliters of aqueous ethanol (10%) wa...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/31.6.342

    authors: Sokoro A,Lehotay D,Eichhorst J,Treble R

    更新日期:2007-07-01 00:00:00

  • Measurement of trazodone using solid-phase extraction and wide-bore capillary gas chromatography with nitrogen-selective detection.

    abstract::A method for the determination of the antidepressant drug trazodone is presented. 8-Hydroxyloxapine is used as the internal standard. A simple solid-phase extraction procedure utilizing disposable reversed-phase C18 columns is described. Samples are analyzed by gas chromatography with nitrogen-selective detection usin...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/12.3.150

    authors: Rifai N,Levtzow CB,Howlett CM,Phillips JC,Parker NC,Cross RE

    更新日期:1988-05-01 00:00:00

  • Further evidence for the presence of GHB in postmortem biological fluid: implications for the interpretation of findings.

    abstract::Analysis and interpretation of the findings for the drug of abuse gamma hydroxybutyric acid (GHB) in fatalities has become very problematic. This is primarily because of variable data in postmortem biological fluids resulting from the endogenous nature of the compound, possible postmortem production, and varying metho...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/28.1.20

    authors: Elliott SP

    更新日期:2004-01-01 00:00:00

  • Prescription Opioids. IV: Disposition of Hydrocodone in Oral Fluid and Blood Following Single-Dose Administration.

    abstract::The Substance Abuse and Mental Health Services Administration (SAMHSA) is currently evaluating hydrocodone (HC) for inclusion in the Mandatory Guidelines for Federal Workplace Drug Testing Programs. This study evaluated the time course of HC, norhydrocodone (NHC), dihydrocodeine (DHC) and hydromorphone (HM) in paired ...

    journal_title:Journal of analytical toxicology

    pub_type: 临床试验,杂志文章

    doi:10.1093/jat/bkv050

    authors: Cone EJ,DePriest AZ,Heltsley R,Black DL,Mitchell JM,LoDico C,Flegel R

    更新日期:2015-09-01 00:00:00

  • Urinary excretion of alpha-hydroxytriazolam following a single dose of halcion.

    abstract::As an approved medicinal product and reportedly an abused substance that have been associated with death and "considered to be a factor...of impaired driving, sexual assault, and other violent crimes", triazolam is controlled at the same level (Level III) as flunitrazepam in Taiwan. Alleged misuses of this substance h...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/29.2.118

    authors: Lin DL,Huang TY,Liu HC,Yin RM

    更新日期:2005-03-01 00:00:00

  • Simultaneous determination of amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), and methylenedioxyethylamphetamine (MDEA) enantiomers by GC-MS.

    abstract::A method is described for the simultaneous determination of the ratio of l- and d-enantiomers of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) in urine. The assay uses liquid-liquid extraction followed by deriv...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/23.6.518

    authors: Hensley D,Cody JT

    更新日期:1999-10-01 00:00:00

  • Evaluation of four immunoassay screening kits for the detection of benzodiazepines in urine.

    abstract::The identification of benzodiazepines (BZD) in biological fluids can be a challenging process. The large number of various BZD in pharmaceutical distribution, with similar core structures, and individual metabolic profiles all contribute to a complicated and time-consuming analysis. The purpose of the current study wa...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/32.6.433

    authors: DeRienz RT,Holler JM,Manos ME,Jemionek J,Past MR

    更新日期:2008-07-01 00:00:00

  • Impact of lowering confirmatory test cutoff value in pre-enlistment urine cannabinoids screening: about five years' experience in the French Gendarmerie.

    abstract::The guidelines for screening of urinary cannabinoids require that all specimens testing positive should be confirmed by gas chromatography-mass spectrometry at a confirmatory test cutoff value of 15 ng/mL of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH). To assess the impact of lowering the confirmatory test cuto...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/bks067

    authors: Lecompte Y,Perrin M,Salle S,Roussel O

    更新日期:2012-10-01 00:00:00

  • Death by arsenic: a comparative evaluation of exhumed body tissues in the presence of external contamination.

    abstract::External contamination of hair or nails by inorganic arsenic compounds cannot effectively be removed with H2O or dilute HCl. The use of a modified Gutzeit apparatus allowed to establish or rule out external contamination. It was found that contaminated samples will generate large amounts of arsine gas when treated wit...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/7.5.216

    authors: Pirl JN,Townsend GF,Valaitis AK,Grohlich D,Spikes JJ

    更新日期:1983-09-01 00:00:00

  • Stability and Degradation Pathways of Different Psychoactive Drugs in Neat and in Buffered Oral Fluid.

    abstract::Sampling and drug stability in oral fluid (OF) are crucial factors when interpreting forensic toxicological analysis, mainly because samples may not be analyzed immediately after collection, potentially altering drug concentrations. Therefore, the stability of some common drugs of abuse (morphine, codeine, 6-monoacety...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/bkz114

    authors: Marchei E,Malaca S,Graziano S,Gottardi M,Pichini S,Busardò FP

    更新日期:2020-07-31 00:00:00

  • Urinary Kinetics of Heroin Metabolites in Pigs Shortly After Intake.

    abstract::In previous experimental studies on heroin metabolites excretion in urine, the first sample was often collected a few hours after intake. In forensic cases, it is sometimes questioned if a positive urine result is expected e.g., 30 min after intake. The aim of this study was to investigate urinary excretion of heroin ...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/bkx017

    authors: Høiseth G,Gottås A,Berg T,Arnestad M,Halvorsen PS,Bachs LC

    更新日期:2017-06-01 00:00:00

  • Two cases of fatal intoxication due to tranylcypromine overdose.

    abstract::Two cases of death following the ingestion of tranylcypromine are presented. High concentrations of tranylcypromine were determined in blood, urine, and liver by gas-liquid chromatography. Tranylcypromine was extracted from buffered blood with n-butyl chloride. The evaporated extract was derivatized with trifluoroacet...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/15.1.38

    authors: Boniface PJ

    更新日期:1991-01-01 00:00:00

  • Selective determination of amitriptyline and nortriptyline in human plasma by HPLC with ultraviolet and particle beam mass spectrometry.

    abstract::A selective, sensitive, and reliable method was devised to determine concentrations of amitriptyline and its major metabolite, nortriptyline, in human plasma using high-performance liquid chromatography (HPLC) combined with UV and particle beam mass spectrometry (PBMS). Amitriptyline and nortriptyline were effectively...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/21.3.185

    authors: Kudo K,Jitsufuchi N,Imamura T

    更新日期:1997-05-01 00:00:00

  • Lethal poisoning with ethiofencarb and ethanol.

    abstract::Ethiofencarb is one of the carbamate compounds, which are, in general, less toxic than organophosphorus insecticides. This is due to their reversible acetylcholinesterase inhibition and relative inability to cross the blood-brain barrier. Generally, ethiofencarb is regarded to be of low toxicity (LD(50) > 200 mg/kg); ...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/33.7.389

    authors: Al-Samarraie MS,Karinen R,Rognum T,Hasvold I,Opdal Stokke M,Christophersen AS

    更新日期:2009-09-01 00:00:00

  • Long-Term Blood Alcohol Stability in Forensic Antemortem Whole Blood Samples.

    abstract::The effect of long-term room temperature storage on the stability of ethanol in whole blood specimens was investigated. One hundred and seventeen preserved whole blood case samples (110 of 117 with two tubes of blood in each case) were used for this study. One tube from each case was initially tested for blood alcohol...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/bkv037

    authors: Tiscione NB,Vacha RE,Alford I,Yeatman DT,Shan X

    更新日期:2015-07-01 00:00:00

  • Metabolism and the urinary excretion profile of the recently scheduled designer drug N-Benzylpiperazine (BZP) in the rat.

    abstract::The metabolism of N-benzylpiperazine (BZP), a recently scheduled designer drug, in the rat has been studied by analyzing its urinary metabolites. p-Hydroxy-BZP (p-OH-BZP) was unequivocally identified as the main metabolite along with a minor metabolite m-hydroxy-BZP (m-OH-BZP), using gas chromatography-mass spectromet...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/30.1.38

    authors: Tsutsumi H,Katagi M,Miki A,Shima N,Kamata T,Nakajima K,Inoue H,Kishi T,Tsuchihashi H

    更新日期:2006-01-01 00:00:00

  • Computer-aided screening for hallucinogenic and stimulant amphetamines with gas chromatography-Fourier transform infrared spectroscopy (GC-FTIR).

    abstract::An expert system applied as a screening test for amphetamine analogues found in recreational-drug exhibits (tablets or powders) is described. The knowledge base defining the reference Fourier transform infrared spectroscopic (FTIR) spectral patterns has been built according to criteria encompassing toxicological, phar...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/25.1.45

    authors: Praisler M,Dirinck I,Van Bocxlaer JF,De Leenheer AP,Massart DL

    更新日期:2001-01-01 00:00:00

  • Flecainide intoxication.

    abstract::A fatal case attributed to flecainide intoxication is presented. Quantitation was by capillary gas chromatography with nitrogen-phosphorus detection. The flecainide concentration in the blood was 13 mg/L as compared to a therapeutic range in serum of 0.2-1.0 mg/L. Flecainide concentrations in other specimens were as f...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/14.5.335

    authors: Levine B,Chute D,Caplan YH

    更新日期:1990-09-01 00:00:00

  • A new specific method to detect cyanide in body fluids, especially whole blood, by fluorimetry.

    abstract::This study shows a simple, rapid, and specific method for the quantitative determination of cyanide ion in body fluids, especially blood, by fluorimetry. It is based upon the transformation of cyanide ion into hydrocyanic acid, which then reacts with 2,3-naphthalenedialdehyde and taurine in a self-contained system. Th...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/22.5.363

    authors: Felscher D,Wulfmeyer M

    更新日期:1998-09-01 00:00:00

  • A comparison of Roche Kinetic Interaction of Microparticles in Solution (KIMS) assay for cannabinoids and GC-MS analysis for 11-nor-9-carboxy-delta9-tetrahydrocannabinol.

    abstract::In this study, we investigated the effectiveness of the Roche Kinetic Interaction of Microparticles in Solution (KIMS) screening assay for cannabinoid metabolites. Urine specimens (N = 1689) were collected during elimination of cannabinoids from 25 subjects with a history of marijuana use. Specimens were analyzed conc...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/25.7.559

    authors: Lyons TP,Okano CK,Kuhnle JA,Bruins MR,Darwin WD,Moolchan ET,Huestis MA

    更新日期:2001-10-01 00:00:00

  • Applying quantitative structure-activity relationship (QSAR) methodology for modeling postmortem redistribution of benzodiazepines and tricyclic antidepressants.

    abstract::Postmortem redistribution (PMR) constitutes a multifaceted process, which complicates the interpretation of drug concentrations by forensic toxicologists. The present study aimed to apply quantitative structure-activity relationship (QSAR) analysis for modeling PMR data of structurally related drugs, 10 benzodiazepine...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/bku025

    authors: Giaginis C,Tsantili-Kakoulidou A,Theocharis S

    更新日期:2014-06-01 00:00:00

  • Trazodone overdose: report of two cases.

    abstract::Two cases of overdose due to ingestion of trazodone are described. In one case, blood collected several hours following ingestion of an estimated 4 or more grams contained a trazodone concentration of 25.7 mg/L. Recovery was uneventful. The second case did not survive and death was attributed to the ingestion of multi...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/8.2.91

    authors: Root I,Ohlson GB

    更新日期:1984-03-01 00:00:00

  • An HPLC method for the quantitation of quinidine and its metabolites in plasma: an application to a quinidine-phenytoin drug interaction study.

    abstract::A rapid and simple method is described for the separation of quinidine (Q), its metabolites 3-hydroxyquinidine (30HQ) and 2'oxoquinidinone (QD) as well as the quinidine salt contaminant, dihydroquinidine (DHQ) in plasma by high pressure liquid chromatography (HPLC). A silica column was used with methanol: 1 N ammonium...

    journal_title:Journal of analytical toxicology

    pub_type: 杂志文章

    doi:10.1093/jat/6.3.153

    authors: Pershing LK,Peat MA,Finkle BS

    更新日期:1982-05-01 00:00:00