Method development for simultaneous determination of amphetamine type stimulants and cannabinoids in urine using GC–MS

Kim, Seon Yeong; Kim, Jin Young; Kwon, Woonyong; In, Moon Kyo; Kim, Young Eun; Paeng, Ki‐Jung

doi:10.1016/j.microc.2013.04.004

Cited by 36 publications

(25 citation statements)

References 15 publications

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“…A mphetamine-type stimulants (ATS) are among the illicit stimulant drugs that are most often used worldwide [1]. ATS act by inducing the release of monamines from nerve terminals in the brain.…”

Section: Introductionmentioning

confidence: 99%

“…In recent years, an increasing number of analytical methodologies based on high-performance liquid chromatography mass spectrometry (HPLC-MS) [3,4] and gas chromatography mass spectrometry (GC-MS) [1,5] have been developed to detect ATS. However, most of these methods involve timeconsuming procedures, especially tedious and elaborate sample pretreatment that includes liquid-liquid extraction, solid phase extraction, and sometimes derivatization to enhance sensitivity [5].…”

Section: Introductionmentioning

confidence: 99%

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Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Crevelin

Salami

Alves

et al. 2016

J. Am. Soc. Mass Spectrom.

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Time Intensity Q1Q2 CID ASAP Probe Corona ConeAbstract. Amphetamine-type stimulants (ATS) are among illicit stimulant drugs that are most often used worldwide. A major challenge is to develop a fast and efficient methodology involving minimal sample preparation to analyze ATS in biological fluids. In this study, a urine pool solution containing amphetamine, methamphetamine, ephedrine, sibutramine, and fenfluramine at concentrations ranging from 0.5 pg/mL to 100 ng/mL was prepared and analyzed by atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) and multiple reaction monitoring (MRM). A urine sample and saliva collected from a volunteer contributor (V1) were also analyzed. The limit of detection of the tested compounds ranged between 0.002 and 0.4 ng/mL in urine samples; the signal-to-noise ratio was 5. These results demonstrated that the ASAP-MS/MS methodology is applicable for the fast detection of ATS in urine samples with great sensitivity and specificity, without the need for cleanup, preconcentration, or chromatographic separation. Thus ASAP-MS/MS could potentially be used in clinical and forensic toxicology applications.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Crevelin

Salami

Alves

et al. 2016

J. Am. Soc. Mass Spectrom.

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“…Logo, o valor de LD foi 1 ng mL -1 . Determinação de THC-COOH por UPLC-MS-MS o limites de detecção foi de 3 ng mL -1 e valores similares ao desse estudo foi encontrado por GC-MS (0,86 ng mL -1 ) [5]. Com a técnica de extração por SPE e análise por LC-MS-MS, o LD foi de 2 ng mL -1 [22].…”

Section: Figura 5 Teste De Seletividade Cromatogramas De íOns Totaiunclassified

“…Os canabinóides mais abundantes são o THC, seu precursor canabidiol e o canabinol, um produto de decomposição formado espontaneamente a partir do THC [2] As principais matrizes para a análise de canabinóides em usuários são: cabelo [3], sangue [4] e urina [5]. Esta última é a amostra biológica mais utilizada para identificação do uso recente da maconha, por ser mais fácil de coletar, não invasiva e as concentrações e seus produtos de biotransformação são relativamente altas quando comparadas com as demais amostras biológicas [5]. Nessa matriz, o principal metabólito do Δ 9 -tetraidrocanabinol é o composto não psicoativo 11-nor-9-carboxi-Δ 9 -tetraidrocanabinol (11-nor-9-carboxy-Δ 9 -tetrahydrocannabinol, THC-COOH), que é excretado em urina e constitui evidência de uso recente da Cannabis [6].…”

Section: Introductionunclassified

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Aplicação da microextração líquido-líquido dispersiva com solidificação da gota orgânica flutuante para determinação de 11-nor-9-carboxi-Δ9-tetraidrocanabinol em urina humana com derivação on-line no sistema de injeção cromatográfico

Dórea

Gomes²,

Prata³

et al. 2017

Scientia Plena

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Determinação de 11-nor-9-carboxi-Δ 9 -tetraidrocanabinol em urina humana por microextração líquido-líquido dispersiva com solidificação da gota orgânica flutuante e derivação online no sistema de injeção cromatográficoDetermination of 11-nor-9-carboxy-δ9-tetrahydrocannabinol in human urine by dispersive liquid-liquid microextraction with solidification of a floating organic drop and on-line derivatization in the injection system chromatographic H. A Cannabis sativa é a droga de abuso mais consumidas no mundo. Devido à baixa concentração dos metabólitos em amostras complexas, novas técnicas de extração estão sendo estudadas. O objetivo desse trabalho foi aplicar a Microextração Líquido-Líquido Dispersiva com Solidificação da Gota Orgânica Flutuante (DLLME-SFO) para determinar o 11-nor-9-carboxi-Δ 9 -tetraidrocanabinol (THC-COOH) em urina humana. Além disso, estabelecer um procedimento on line para a derivação do metabólito no injetor cromatográfico. O analito foi extraído da urina depois da hidrólise alcalina do glicuronídeo, usando o solvente de extração 1-dodecanol (30 µL) e o metanol (200 µL) como dispersor. NaCl 1% foi adicionado e o tempo de extração foi de 5 min. A melhor proporção entre BSTFA:extrato para derivação on line do THC-COOH foi 2:2, injetor operado no modo split 1:20 e temperatura de 240 °C. O extrato foi analisado por cromatografia gasosa acoplada a espectrometria de massas no modo tandem (GC-MS/MS), depois da definição dos ions pais (m/z), da energia de excitação (modo ressonante) e dos ions filhos para a quantificação e confirmação (m/z) do canabinóide e do padrão interno deuterado. Os limites de detecção (LD) e de quantificação (LQ) foram 1 e 10 ng mL -1 , respectivamente. O método analítico proposto apresentou vantagens com relação à sensibilidade, especificidade, linearidade e custo com relação à extração em fase sólida, assim como é adequado à química verde e seus limites são apropriados para analisar THC-COOH em urina humana.Palavras-chave: THC-COOH, urina, DLLME-SFO.Cannabis sativa is the most used drug in the world. Due to the low concentration of metabolites in complex samples, new extraction techniques are being studied. The objective of this study was to develop an analytical method by applying the technique of Dispersive Liquid-Liquid MicroextractionSolidification of a Floating Organic Drop (DLLME-SFO) to determine 11-nor -9-carboxyl -Δ 9 -tetrahydrocannabinol (THC-COOH) in human urine sample. In addition, it was established an online procedure for derivatisation of the metabolite in the chromatographic injector. After of the glucuronide alkaline hydrolysis, the analyte was extracted with 1-dodecanol (30 µL) and methanol (200 µL), as extraction and dispersive solvents, respectively, addition of 1 % NaCl and 5 min to extraction time. The best proportion between BSTFA:extract for on line derivatization of the THC-COOH was 2:2, the split was 1:20 and 240 °C for temperature. The extract was analyzed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS), after definition ...

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High‐throughput doping control analysis of 28 amphetamine‐type stimulants in equine plasma using hydrophilic interaction liquid chromatography–tandem mass spectrometry

You

Guan

D'Ippolito

et al. 2018

Drug Testing and Analysis

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A hydrophilic interaction liquid chromatography-tandem mass spectrometry method (HILIC-MS/MS) was developed for the simultaneous determination of 28 amphetamine-type stimulants (ATSs) in equine plasma for doping control analysis. In this method, stimulants were recovered from equine plasma by liquid-liquid extraction (LLE) at pH 9.5 using methyl tert-butyl ether and detected on a Thermo Finnigan triple quadrupole mass spectrometer operating in positive-ion mode electrospray ionization.All stimulants were eluted within 7 minutes and baseline separation was achieved for isomeric and isobaric compounds using HILIC chromatography. Extraction efficiency was greater than 80% and matrix effect was acceptable for most stimulants. The limit of detection (LOD) was in the range of 10-50 pg/mL and the lower limit of quantification (LLOQ) was in the range of 50-100 pg/mL. Quadratic regression was employed for quantification and the dynamic range of quantification was 50-10000 pg/mL. Confirmatory analysis criteria were established using product ion ratios and retention time. The limit of confirmation (LOC) was in the range of 20-100 pg/mL. Stability study results indicated that some stimulants were unstable in equine plasma at room temperature and 4°C. However, all the stimulants studied were stable at −20°C and − 80°C for the 6 month study period.

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Method development for simultaneous determination of amphetamine type stimulants and cannabinoids in urine using GC–MS

Cited by 36 publications

References 15 publications

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Aplicação da microextração líquido-líquido dispersiva com solidificação da gota orgânica flutuante para determinação de 11-nor-9-carboxi-Δ9-tetraidrocanabinol em urina humana com derivação on-line no sistema de injeção cromatográfico

High‐throughput doping control analysis of 28 amphetamine‐type stimulants in equine plasma using hydrophilic interaction liquid chromatography–tandem mass spectrometry

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