Qualitative identification of imidacloprid in postmortem animal tissue by gas chromatography-tandem mass spectrometry.

During an avian mass mortality event investigation at the National Fish and Wildlife Forensic Laboratory in Ashland, OR, imidacloprid became an insecticide of concern. A qualitative analytical toxicology screen of seeds, plucks (tongue, esophagus, and trachea), and ventricular contents was requested. A method for the extraction and qualitative analysis of the insecticide in animal tissues was therefore developed. The procedure relies on a combined Food Emergency Response Network (FERN) and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) approach to sample extraction followed by qualitative analysis by gas chromatography-tandem mass spectrometry. Since imidacloprid is not amenable to the conditions of gas chromatography, a trimethylsilyl derivative was created and characterized. Proposed mechanisms for the creation of this derivative and its mass spectrum are described. The imidacloprid-trimethylsilyl (TMS) derivative was detected in all samples submitted.

Analysis of Acetyl Fentanyl in Postmortem Specimens by Gas Chromatography-Mass Spectrometry (GC-MS): Method Validation and Case Report.

In 2013, the Centers for Disease Control and Prevention released a warning regarding a new recreational drug, acetyl fentanyl. Acetyl fentanyl is a µ-opioid receptor agonist, and its pharmacological effects include euphoria, altered mood, miosis and central nervous system depression. The objective of this report was to develop a sensitive and specific method for the quantitation of acetyl fentanyl by gas chromatography-mass spectrometry in postmortem casework. Acetyl fentanyl was isolated from biological matrices using solid-phase extraction and acetyl fentanyl-13C6 was employed as an internal standard. The method was validated utilizing the Scientific Working Group for Forensic Toxicology's published method validation parameters, and the biological matrices used for analysis were postmortem blood and urine. In addition to the quantitation of acetyl fentanyl, a demographic study of cases obtained from the Rhode Island Office of State Medical Examiners and the University of Florida Health Pathology Laboratories-Forensic Toxicology Laboratory was performed to examine potential risk factors for acetyl fentanyl use. The results from this study found that the blood concentrations in these individuals ranged from 17 to 945 ng/mL. This suggests acetyl fentanyl is less potent than its prototype drug, fentanyl and requires an increased dose to achieve its desired effects. The demographic analysis indicated white males aged 21-40 years and individuals with a previous history of drug use have the highest risk for acetyl fentanyl abuse.

A Gas Chromatography-Triple Quadrupole Mass Spectrometry Assay for the Quantification of Opiates in Human Blood Samples.

A simplified protein precipitation method in combination with gas chromatography-triple quadrupole mass spectrometry (GC-MS-MS) analysis was developed and validated for the simultaneous determination of codeine, morphine, 6-acetylmorphine (6-MAM), hydrocodone and hydromorphone in human blood samples. A protein precipitation with 10% trichloroacetic acid followed by solid-phase extraction using a mixed-mode cartridge was used to separate the analyte from the blood samples. A BSTFA + 1% TMCS was used for derivatization of opiates prior to the analysis. Codeine-D3, morphine-D3, 6-acetylmorphine-D3 and hydrocodone-D6 were used as internal standards. The GC-MS-MS was operated under multiple-reaction monitoring mode using electron ionization technique. The transition ions used for quantitation were 371 → 234 for codeine, 429 → 146 for morphine, 399 → 287 for 6-MAM, 299 → 228 for hydrocodone and 357 → 314 for hydromorphone. The method was linear over the concentration range 2.5-1000 ng/mL for all analytes, except hydrocodone which was linear over 5-1000 ng/mL with a correlation coefficient (r2) = 0.99. The limit of detection was 1.0 ng/mL for all compounds except hydrocodone which was 2.5 ng/mL. The limit of quantitation was 2.5 ng/mL for all compounds except hydrocodone which was 5.0 ng/mL. The precision (% RSD) was within 1.26-14.81 and the accuracy (% Bias) was within -6.29-10.93% for all compounds. The method successfully analyzed morphine (305 ng/mL) and 6-acetylmorphine (6-MAM) (2.3 ng/mL) in a human blood sample received from an opiate user.

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

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.

Simultaneous Determination of Amphetamine-Related New Psychoactive Substances in Urine by Gas Chromatography-Mass Spectrometry.

Despite the efforts to prevent the spread of new psychoactive substances (NPS) such as synthetic amphetamine derivatives, it is apparent that newer types of NPS are still emerging on the market in recent years. Due to high potential for their abuse, reliable analytical methods are required to determine these substances in biological samples. The objective of this study was to develop and validate the gas chromatography-mass spectrometric (GC-MS) method for the simultaneous determination of 13 amphetamine-related NPS (amphetamine; AP, 4-fluoroamphetamine; 4FA, methamphamine; MA, 4-fluoromethamphetamine; 4FMA, 4-chloroamphetamine; 4CA, para-methoxyamphetamine; PMA, 4-chloromethamphetamine; 4CMA, 6-(2-aminopropyl)benzofuran; 6APB, 4-methylenedioxyamphetamine; MDA, para-methoxymethamphetamine; PMMA, 6-(2-methylaminopropyl)benzofuran; 6MAPB, 3,4-methylenedioxymethamphetamine; MDMA, 5,6-methylenedioxy-2-aminoindane; MDAI) in urine. The analytes were extracted at pH 7.4 by liquid-liquid extraction prior to their trifluoroacetyl derivatives and then analyzed by GC-MS. The validation parameters included selectivity, linearity, lower limits of quantification (LLOQ), intra and interday precision and accuracy, recovery and stability. The linear ranges were 2-100 ng/mL for AP, 4FA, 4FMA, 4CA, PMA, 6APB, MDA, and MDAI, 2-250 ng/mL for 4CMA, PMMA, and 6MAPB and 25-1,000 ng/mL for MA and MDMA, with acceptable coefficients of determination (r2 > 0.9963). The intra and interday precision were within 11.9 and 12.5%, while the intra and interday accuracies ranged from -10.6% to 13.0% and -11.0% to 6.8% for the nominal concentration at all studied levels, respectively. The LLOQs for each analyte were 2.0-25 ng/mL. The recoveries ranged from 69.3% to 96.4%. The short- and long-term variations of the analytes in urine were lower than 8.5 and 12.7%, indicating that the analytes are stable at least for 16 h at room temperature and for 7 days at 4°C, respectively. The applicability of the method was examined by analyzing urine samples from drug abusers and was determined to be effective for detecting multiple drug use.

Determinação de club dugs em sangue total por cromatografia líquida acoplada a espectrometria de massas com analisador hí­brido quadrupolo-tempo de voo (LC-QTOF-MS) / Determination of club drugs in whole blood by liquid chromatography coupled with mass spectrometry with hybrid quadrupole time-of-flight mass analyzer (LC-QTOF)

As chamadas club drugs compreendem um vasto grupo de substâncias frequentemente utilizadas em bares, festas e raves, com a finalidade de intensificar o contato social e a estimulação sensorial. Englobam desde substâncias sintéticas comumente conhecidas, como a anfetamina, a metanfetamina, o MDMA, até moléculas de surgimento mais recente, denominadas novas substâncias psicoativas. Isoladas ou associadas a outras drogas, é possível que sejam causa de morte per se, ou que predisponham o usuário a envolver-se em situações potencialmente fatais, sendo necessário que os órgãos de Perícia Criminal (Institutos Médico Legais e Institutos de Criminalística) estejam aptos a detectar e quantificar essas substâncias em amostras biológicas. O presente trabalho teve como objetivo desenvolver um método analítico para identificação e quantificação de club drugs em sangue total, utilizando cromatografia líquida acoplada a espectrometria de massas com analisador híbrido quadrupolotempo de voo (LC-QTOF). Após o desenvolvimento do método, este foi validado utilizando as diretrizes do guia de validação do Scientific Working Group for Forensic Toxicology (SWGTOX), sendo analisados de linearidade, limite de detecção, limite de quantificação, efeito matriz, precisão intradia, precisão interdia, exatidão e integridade de diluição, além de recuperação e eficiência do processo. O método desenvolvido compreendeu a determinação de MDA, MDMA, 2C-B, DOB, cetamina, mCPP, cocaína e cocaetileno. Amostras provenientes de casos reais de morte não natural, oriundas do Instituto Médico Legal Aristoclides Teixeira de Goiânia - GO foram analisadas pelo método desenvolvido. 56 casos foram selecionados, em sua maioria com histórico de morte por projétil de arma de fogo e acidente de transito. Das 56 amostras analisadas, 28,5% (n=16) foram positivas para cocaína e/ou cocaetileno. As demais substâncias pesquisadas não foram encontradas nas amostras

Club drugs are a large group of substances consumed in pubs, parties and raves, aiming to intensify social contact and sensorial stimulation. The term comprises largely known substances such as amphetamine, methamphetamine, 3,4-methylenodioxymethamphetamine (MDMA), as well as so-called new psychoactive substances, which are synthetic drugs recently developed or recently introduced in drug market. Club drugs can be taken alone, combined with each other or, most frequently, with alcohol or other commonly abused drugs such as cocaine. In any of these situations, club drugs can possibly be the cause of death or potentialize the involvement of the user with crime and potentially fatal behavior. Thus, official organisms in charge of criminal investigation must be capable of identifying and quantifying these substances in biological samples. The present work aimed the development of an analytical method to identify and quantify club drugs in whole blood, using liquid chromatography - mass spectrometry with hybrid analyzer quadrupole - time of flight (LC-QTOF). After analytical development, the method was validated according to do Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines, evaluating linearity, limit of detection, limit of quantification, matrix effect, precision, intermediate precision, bias and dilution integrity, besides recovery and process efficiency. The developed method comprised MDA, MDMA, 2C-B, DOB, ketamine, mCPP, cocaine and cocaethylene determination. Real samples related to non-natural deaths were collected at Institute of the Legal Medicine Aristoclides Teixeira, Goiânia, Goiás, Brazil, and analyzed by the developed method. 56 cases were selected, most of them related to fire gun injury and traffic events, 28,5% (n=16) of them being positive for cocaine and/or cocaethylene. None of the other drugs comprised in the analysis were detected in these samples

Redistribuição postmortem de antidepressivos e seus produtos de biotransformação em tecidos biológicos humanos / Postmortem redistribution of antidepressants and their metabolites in human biological tissues

Os antidepressivos pertencem a uma importante classe de medicamentos investigados na toxicologia forense. Em casos de amostras provenientes de cadáveres, o intervalo entre o óbito e a obtenção da espécie biológica pode proporcionar a redistribuição postmortem destes fármacos. Com o objetivo de elucidar esse fenômeno, métodos analíticos foram desenvolvidos e aplicados utilizando sangue total (ST), humor vítreo (HV) e fígado. Para as amostras de ST e HV, o método de extração escolhido e validado foi a microextração em fase líquida (LPME) trifásica. Fibras ocas constituídas de polipropileno, com a extensão de 8 cm cada, foram tratadas com o solvente orgânico dodecano (fase orgânica), resultando em um membrana com permeabilidade seletiva. No lúmen destas fibras, adicionou-se ácido fórmico 0,1 mol/L (fase aceptora). Em frasco de fundo chato com 5 mL de capacidade, pipetou-se 3,5 mL de NaOH 0,1 mol/L (fase doadora) e 0,5 mL de ST ou HV. Ao término da extração, as amostras foram introduzidas no GC-MS, sem a necessidade de reações de derivatização. O estudo com ST contemplou os antidepressivos amitriptilina (AMI), nortriptilina (NTR), imipramina (IMI), desipramine (DES), clomipramina (CLO), desmetilclomipramina (DMC), fluoxetina (FLU) e norfluoxetina (NFL). Os limites de quantificação para estas substâncias ficaram inferiores aos níveis terapêuticos (20 ng/mL). As médias dos coeficientes de variação intradia e interdia foram, respectivamente, de 9,7 e 9,8%. As curvas de calibração apresentaram linearidade entre as concentrações de 20 até 1200 ng/mL. A validação do parâmetro integridade da diluição assegurou a mensuração de quantidades superiores ao limite apresentado na curva de calibração. O método foi aplicado em sete amostras reais postmortem e em apenas um caso foi observada uma diferença significativa (300%) entre os valores quantificados no ST periférico e central. Os antidepressivos tricíclicos AMI, NTR, IMI e DES foram avaliados no HV e o efeito matriz foi detectado para os dois últimos analitos. O método foi otimizado e validado utilizando solução salina adicionada de AMI e NTR. O limite de detecção igual a 5 ng/mL, foi obtido com a redução da voltagem da fonte de íons do espectrômetro de massa para 50 eV. Coeficientes de variação foram inferiores a 15%. Os procedimentos validados foram aplicados em seis amostras reais de HV. A relação encontrada entre os valores obtidos no ST periférico e HV foi de aproximadamente 0,1. A extração acelerada por solvente (ASE) e, posteriormente, a extração em fase sólida (SPE) foram as técnicas de separação dos analitos da matriz fígado. Ao término das citadas extrações, os antidepressivos foram analisados no GC-MS. Para esta matriz sólida, são necessários mais estudos, pois os valores encontrados nos ensaios analíticos estão em desacordo com as diretrizes utilizadas na validação dos métodos

Antidepressants belong to an important class of drugs investigated in forensic toxicology. In cases of samples from corpses, the interval between death and obtaining the biological specimens can provide the postmortem redistribution of these drugs. Aiming to elucidate this phenomenon, analytical methods were developed and applied using whole blood (WB), vitreous humor (VH) and liver. For samples of WB and HV, the extraction method chosen and validated was the three-phase liquid phase microextraction (LPME). Hollow fibers consist of polypropylene, with a length of 8 cm each were treated with dodecane organic solvent (organic phase) resulting in a membrane with selective permeability. Into the lumen of these fibers was added formic acid 0.1 mol/ L (acceptor phase). In the vial containing 3.5 mL of NaOH 0.1 mol / L (donor phase) was spiked 0.5 ml of biological fluids (WB or VH). Subsequently, the samples were injected in GC-MS without derivatization reactions. The study of the ST included antidepressants amitriptyline (AMI), nortriptyline (NTR), imipramine (IMI), desipramine (DES), clomipramine (CLO), desmethylclomipramine (DMC), fluoxetine (FLU) and norfluoxetine (NFL). The quantification limits for these substances were below the therapeutic levels (20 ng / ml). The mean coefficients of variation and separate intradays were respectively 9.7 and 9.8%. The calibration curves showed linearity between concentrations of 20 to 1200 ng / mL. The validation of the integrity of the dilution parameter assured measurement higher than the limit shown in the calibration curve quantities. The method was applied to seven real postmortem samples and in one case a significant difference (300%) between the measured values in the peripheral and central ST was observed. The tricyclic antidepressants AMI, NTR, IMI and DES were evaluated in VH and the matrix effect was detected in the last two analytes. The method was optimized and validated using saline spiked AMI and NTR. The limit of detection (5 ng/ml) was obtained by reducing the voltage of the ion source of the mass spectrometer 50 eV. Coefficients of variation were below 15%. The procedures were validated in six real samples of HV. The relationship found between the values obtained in the peripheral ST and HV was approximately 0.1. Accelerated solvent extraction (ASE) and subsequently the solid phase extraction (SPE) were the techniques of separation of analytes liver matrix. At the end of the cited extractions, antidepressants were analyzed in GC-MS. To this solid tissue, further studies are needed, because the values found in the analytical tests were not in accordance with the guidelines used in the validation of the methods

Development of application protocols of the Emit® II Plus 6-Acetylmorphine Assay on the ADVIA® 1800 and 2400 Chemistry Systems.

New application protocols for the Emit(®) II Plus 6-Acetylmorphine Assay for human urine screening have been developed on the ADVIA(®) 1800 and 2400 Chemistry Systems. Precision was evaluated at the cutoff and ±25% controls. Recovery and linearity were studied by spiking 6-acetylmorphine (6-AM) into human urine pools. Method comparison was evaluated using urine specimens and the results were compared to those obtained from the predicate Analyzer (V-Twin(®)). Cross-reactivity with structurally related drugs was assessed at high cross-reactant concentrations. Potential interferences were assessed in the presence of 7.5 and 12.5 ng/mL of 6-AM. The qualitative repeatability coefficients of variation (CV's) ranged from 0.40 to 0.90% and the within-lab CV's ranged from 1.3 to 3.5%. In analyte units (ng/mL), the repeatability CV's ranged from 1.9 to 4.3% and the within-lab CV's ranged from 3.7 to 6.1%. The limit of detection of the assay was found to be 2.5 ng/mL on both instruments. Recovery was within 20% of expected value. Linearity was 2.5-20 ng/mL. Method comparison showed 100% agreement with the predicate analyzer. The assay had minimal cross-reactivity to structurally related opioids including with morphine, morphine-3-glucuronide, morphine-6-glucuronide. No interference was observed with endogenous interferences.

Calculation and verification of blood ethanol measurement uncertainty for headspace gas chromatography.

An estimate was made of the measurement uncertainty for blood ethanol testing by headspace gas chromatography. While uncertainty often focuses on compliance to a single threshold level (0.08 g/100 mL), the existence of multiple thresholds, related to enhanced sentencing, subject age, or commercial vehicle licensure, necessitate the use of an estimate with validity across multiple specification levels. The uncertainty sources, in order of decreasing magnitude, were method reproducibility, linear calibration, recovery, calibrator preparation, reference material, and sample preparation. A large set of reproducibility data was evaluated (n = 15,433) in order to encompass measurement variability across multiple conditions, operators, instruments, concentrations and timeframes. The relative, combined standard uncertainty was calculated as ±2.7%, with an expanded uncertainty of ±8.2% (99.7% level of confidence, k = 3). Bias was separately evaluated through a recovery study using standard reference material from a national metrology institute. The uncertainty estimate was verified through the use of proficiency test (PT) results. Assigned values for PT results and their associated uncertainties were calculated as robust means (x*) and standard deviations (s*) of participant values. Performance scores demonstrated that the uncertainty estimate was appropriate across the full range of PT concentrations (0.010-0.370 g/100 mL). The use of PT data as an empirical estimate of uncertainty was not examined. Until providers of blood ethanol PT samples include details on how an assigned value is obtained along with its uncertainty and traceability, the use of PT data should be restricted to the role of verification of uncertainty estimates.

Ethanol analysis by headspace gas chromatography with simultaneous flame-ionization and mass spectrometry detection.

Ethanol is the most frequently identified compound in forensic toxicology. Although confirmation involving mass spectrometry is desirable, relatively few methods have been published to date. A novel technique utilizing a Dean's Switch to simultaneously quantitate and confirm ethyl alcohol by flame-ionization (FID) and mass spectrometric (MS) detection after headspace sampling and gas chromatographic separation is presented. Using 100 µL of sample, the limits of detection and quantitation were 0.005 and 0.010 g/dL, respectively. The zero-order linear range (r(2) > 0.990) was determined to span the concentrations of 0.010 to 1.000 g/dL. The coefficient of variation of replicate analyses was less than 3.1%. Quantitative accuracy was within ±8%, ±6%, ±3%, and ±1.5% at concentrations of 0.010, 0.025, 0.080, and 0.300 g/dL, respectively. In addition, 1,1-difluoroethane was validated for qualitative identification by this method. The validated FID-MS method provides a procedure for the quantitation of ethyl alcohol in blood by FID with simultaneous confirmation by MS and can also be utilized as an identification method for inhalants such as 1,1-difluoroethane.

Assessment of response of the Intoxilyzer 8000C to volatiles of forensic relevance in vitro, part I: acetone, isopropanol, and methanol.

The response of the Intoxilyzer 8000C (version approved for evidentiary breath alcohol testing in Canada) to volatile solvents in vitro is described. Acetone, isopropanol, and methanol were prepared as aqueous solutions or dilutions of standard alcohol solution (SAS; 1.21 mg ethanol/mL) to generate apparent blood ethanol concentrations (aBEC) of 50 or 80 mg/dL. Solvent concentrations examined were relevant to clinical or impaired driving scenarios. Replicates of 20 aBEC measurements were made for each mixture and the actuation of the "INTERFERANT DETECT" message (IDM) was noted. Measurements of aqueous acetone (0-40 mg acetone/dL), isopropanol (0-100 mg isopropanol/dL), and methanol (0-100 mg methanol/dL) yielded aBECs of 0, 0-43, and 0-55 mg/dL, respectively. The minimum concentration examined at which the IDM was actuated in 100% of replicates was 25, 30, and 100 mg/dL for acetone, isopropanol, and methanol, respectively. The maximum concentration examined at which the IDM was actuated in none of the replicates was 5, 10, and 50 mg/dL for acetone, isopropanol, and methanol, respectively. In examinations of acetone/isopropanol mixtures in diluted SAS where the IDM was not always actuated, the maximum BEC overestimation was 10 mg/dL. Overall, the potential for significant undetected BEC overestimation is low and may be further reduced through truncation of test results and subject observation.

Análises físicas e químicas de comprimidos de ecstasy apreendidos no município de São Paulo / Physical and chemical analyses of ecstasy tablets seized in São Paulo city

Drug profiling, isto é, a caracterização de amostras de drogas apreendidas no sentido de estabelecer conexões entre apreensões realizadas em diferentes épocas e/ou locais a uma origem comum de produção clandestina, tem sido um objetivo dos órgãos governamentais responsáveis pela prevenção/repressão. Especificamente tratando-se de comprimidos de ecstasy, o conhecimento de suas propriedades físicas e químicas é de relevante importância para discriminar a apreensão de diferentes lotes. Nesse contexto, o presente trabalho propõe uma nova abordagem para estabelecer conexões entre apreensões de comprimidos de ecstasy, por meio da calorimetria exploratória diferencial (DSC), termogravimetria (TG) e difratometria de raios-X (DRX). Também foi realizada a caracterização física de todos os comprimidos (logotipo, coloração, massa, diâmetro e espessura), bem como a identificação/quantificação dos constituintes ativos por cromatografia em fase gasosa acoplada à espectrometria de massas (GC-MS) e o perfil de dissolução in vitro. Além disso, foi desenvolvido um método empregando a extração líquido-líquido para o isolamento da 3,4-metilenodioximetanfetamina (MDMA) dos comprimidos de ecstasy, que posteriormente foi cristalizada para cloridrato de MDMA (MDMA.HCl). Foram analisados dezessete diferentes lotes de comprimidos de ecstasy de diversos logotipos e colorações apreendidos no município de São Paulo, Brasil. Apenas um lote apresentou como única substância ativa a clorofenilpiperazina (CPP). Os outros continham apenas MDMA e o conteúdo de MDMA variou de 29 a 115-mg/comprimido. Os valores de massa dos comprimidos variaram de 143 a 341-mg, a espessura de 3,2 a 5,8-mm e o diâmetro de 7,0 a 9,5-mm. A comparação das curvas obtidas, tanto por calorimetria exploratória diferencial (DSC) como pelos difratogramas de raios-X (DRX), permitiu discriminar aqueles com perfis semelhantes, importante para identificar a origem de produção. O baixo grau de cristalinidade do MDMA.HCl de alguns comprimidos de ecstasy não impediu a caracterização por DSC e DRX. Esses resultados podem ser úteis para a aplicação no trabalho de inteligência forense

Drug profiling or the characterization of seized drug samples to link seizures made at different times and/or locations to their common clandestine origin, has long been a goal of law enforcement agencies. Considering the trafficking of ecstasy tablets, the knowledge of chemical and physical properties is of utmost importance to discriminate between different seizures. In this context this study proposed a new approach to establish links among seizures of ecstasy tablets by using differential scanning calorimetry (DSC), thermogravimetry (TG) and X-ray diffraction (XRD). Besides this characterization, physical appearance (logotype, color, weight, diameter and thickness), identification/quantification of active constituents by gas chromatography/ mass spectrometry (GC/MS) and in vitro drug dissolution assays were performed too. A method employing liquid-liquid extraction was also developed for the isolation of 3,4-methylenedioxymethamphetamine (MDMA) from ecstasy tablets and afterwards MDMA was crystallized to MDMA hydrochloride (MDMA.HCl). Seventeen different lots of various logotypes and colors of confiscated ecstasy tablets from seizures in São Paulo city, Brazil, were analyzed. Chlorophenylpiperazine (CPP) was found only as an active ingredient in one batch. The others tablets contained only MDMA and the content of MDMA varied from 29 to 115-mg/tablet. The weight values of tablets varied from 143 to 341-mg, the thickness from 3,2 to 5,8-mm and the diameter from 7,0 to 9,5-mm. DSC/TG curves and X-ray difratograms of the ecstasy tablets allowed distinguishing those with similar profile, for both techniques, which is important to identify the source of production. The low degree of MDMA.HCl crystallinity of some ecstasy tablets didnt prevent DSC and XRD characterization. These results can be useful for forensic intelligence work application

[Gas chromatography with mass-selective detector in testing blood for amitriptyline and nortriptyline].

The article describes the method of simultaneous detection of amitriptiline and nortriptilin in cadaveric blood using gas chromatography with mass-selective detection. Preparation includes liquid-liquid extraction and derivation with trifluoroacetic anhydride. Nortriptilin threshold of detectability in the blood is 0.02 mcg/ml, amitriptilin one--0.05 mcg/ml. The range of detectability--0.05-3.0 mcg/ml for both compounds. Maximal error of the compounds detectability was under 12.9% for concentrations 0.10 mcg/ml and 10.6% for concentrations 2.0 mcg/ml. The method was tested on expert material in forensic chemical examinations.