A Gas Chromatography–Mass Spectrometry Method for Toxicological Analysis of MDA, MDEA and MDMA in Vitreous Humor Samples from Victims of Car Accidents

Abstract

Vitreous humor (VH) shows excellent potential as a matrix of choice for postmortem analytical toxicology due to the ease of sampling and low metabolic activity. This study demonstrates a simple and rapid analytical method to identify and quantify 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxy-ethylamphetamine in VH. Samples were collected with a simple eye puncture procedure, followed by liquid-liquid extraction and derivatization with heptafluorobutyric anhydride and analysis via gas chromatography-mass spectrometry. The accuracy of the method ranged 97-103%, intra-assay precision was between 4.54 and 9.14% relative standard deviation (RSD) and interassay precision ranged from 6.92 to 10.59% RSD. Limits of detection and quantification ranged from 1.0 to 2.5 ng/mL and 10 ng/mL, respectively. The validated method was successfully applied to detect methylenedioxyamphetamine derivatives in VH samples collected from victims of fatal car crashes.

Alternative matrices in forensic toxicology: a critical review

“…In the literature, there are several SPE-based methods available proposed for extracting drugs from VH specimens [154][155][156][162][163][164][165][166][167][168]. LLE has also been reported and explored for VH samples [169][170][171][172][173][174][175]. Other techniques have been less frequently explored such as microwave assisted extraction [176], disposable pipette extraction [177], supercritical fluid extraction [178], dispersive liquid-liquid microextraction [179] and liquid-phase microextraction (LPME) [180].…”

“…Chromatography coupled to mass spectrometry-based methods have been frequently used due to its high sensitivity, selectivity and accuracy [151]. Gas chromatographic techniques used in separation and analysis of VH samples include GC-MS [154,156,163,164,[167][168][169][170][180][181][182], gas chromatography with nitrogen-phosphorus detector (GC-NPD) [170,177] and GC-FID [159,166]. Gas chromatography coupled to tandem ion trap mass spectrometry (GC-MS/MS) has also been applied in the analysis of cocaine in sheep's VH [183].…”

Determinação De Designer Drugs Em Saliva Por Paper Spray Mass Spectrometry

“…Já para o MDA, o LD e LQ foram 3,42 µg L -1 e 21,66 µg L -1 , respectivamente.Schepens et al33 mostraram valores próximos de LD e LQ para o MDMA (ambos < 5 µg L -1 ) e para o MDA (10 µg L -1 e 25 µg L -1 ) com o método de Cromatografia Liquida acoplada à MS (LC-MS) para rápida confirmação e quantificação de drogas de abuso em saliva sintética. Ishikawa et al34 também mostraram valores próximos de LD e LQ para o MDA, 2,5 µg L -1 e 10 µg L -1 , e para o MDMA, 1 µg L -1 e 10 µg L -1 , em fluídos biológicos utilizando Cromatografia Gasosa acoplada à Espectrometria de Massa (CG-MS). Portanto, o método de MIP-PSI-MS atingiu resultados próximos aos de técnicas clássicas utilizadas para análises de drogas.A Figura 9 demonstra curvas analíticas que correlacionam concentrações reais (quantidades das drogas concentradas na saliva) com concentrações obtidas por MIP-PSI-MS para as drogas MDA e MDMA.…”

Substâncias psicoativas no sangue: métodos de análises toxicológicas e prevalência do uso em pacientes com lesões traumáticas

“…Entretanto, os estudos realizados em âmbito nacional foram realizados de forma observacional e utilizando relatos dos sujeitos incluídos sobre uso de drogas, o que poderia ter causado uma subnotificação do consumo. No âmbito do trânsito, estudo identificou a presença de MDMA, MDA e MDEA em amostras provenientes de motoristas vítimas fatais de acidentes de trânsito 163 . Por outro lado, nos outros dois estudos brasileiros realizados com pacientes atendidos em salas de emergência, o consumo de anfetaminas não foi relatado 154,155 .…”

“…Recovery results were satisfactory for authors when compared to other published methods. Ishikawa et al (2018), analysing ATS from humor vitreous reported a recovery ranging from 47.2 to 81.5% using liquid-liquid technique [26]. Similarly, Hartman et al (2014) also determining amphetamines from blood and plasma published a solidphase technique with extraction efficiency around 50% [32].…”