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3.
MMWR Morb Mortal Wkly Rep ; 68(47): 1096-1100, 2019 Nov 29.
Artigo em Inglês | MEDLINE | ID: mdl-31774740

RESUMO

During August 9-October 31, 2019, 96 patients were classified as having e-cigarette, or vaping, product use-associated lung injury (EVALI) by the Minnesota Department of Health (MDH); other patients are being investigated for case classification and exposures. Among 58 patients interviewed, 53 (91%) reported obtaining tetrahydrocannabinol (THC)-containing products from informal sources such as friends, family members, or in-person or online dealers. Using gas chromatography-mass spectrometry (GCMS), the MDH Public Health Laboratory (PHL) analyzed 46 THC-containing e-cigarette, or vaping, products obtained from 12 EVALI patients for various potential toxicants, including vitamin E acetate, which has recently been detected in some THC-containing products and in samples of lung fluid from EVALI patients (1-4). To explore whether vitamin E acetate is a recently added component in THC-containing products, MDH tested ten products seized by law enforcement in 2018, before the EVALI outbreak, and 20 products seized in 2019, during the outbreak. Twenty-four products obtained from 11 EVALI patients from 2019 contained vitamin E acetate. Among the seized products tested by MDH, none seized in 2018 contained vitamin E acetate, although all tested THC-containing products seized in 2019 tested positive for vitamin E acetate. These chemical analyses of products obtained from EVALI patients and of products intended for the illicit market both before and during the outbreak support a potential role for vitamin E acetate in the EVALI outbreak; however, the number of products tested was small, and further research is needed to establish a causal link between exposure to inhaled vitamin E acetate and EVALI. Collaboration between public health jurisdictions and law enforcement to characterize THC-containing products circulating before the recognition of the EVALI outbreak and during the outbreak might provide valuable information about a dynamic market. These Minnesota findings highlight concerns about e-cigarette, or vaping, products that contain THC acquired from informal sources. Because local supply chains and policy environments vary, CDC continues to recommend not using e-cigarette, or vaping, products that contain THC or any e-cigarette, or vaping, products obtained from informal sources. E-cigarette, or vaping, products should never be used by youths, young adults, or pregnant women.* Until the relationship between inhaled vitamin E acetate and lung health is better characterized, vitamin E acetate should not be added to e-cigarette, or vaping, products.


Assuntos
Sistemas Eletrônicos de Liberação de Nicotina , Legislação de Medicamentos , Lesão Pulmonar/epidemiologia , Vaping/efeitos adversos , Adolescente , Adulto , Idoso , Dronabinol/efeitos adversos , Dronabinol/análise , Feminino , Humanos , Aplicação da Lei , Masculino , Pessoa de Meia-Idade , Minnesota/epidemiologia , Vitamina E/efeitos adversos , Vitamina E/análise , Adulto Jovem
4.
An Acad Bras Cienc ; 91(3): e20190676, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31618414

RESUMO

The aim of this work was to optimize a maceration condition of cannabis (Cannabis sativa L.). A circumscribed central composite experimental design was applied in this work. Temperature and time were varied from 40-80 °C and 30-90 min, respectively. The three responses (i.e., extraction yield, cannabidiol content, and Δ9- tetrahydrocannabinol content) were predicted by computer software. The yield was high when cannabis was macerated using ethanol at high temperature and long duration time. While cannabidiol and Δ9- tetrahydrocannabinol content was high when macerating at a low heating temperature and short duration time. The optimal condition provided the simultaneous high of cannabidiol and Δ9- tetrahydrocannabinol content was 40 °C for 30 min. The prediction was accurate due to low percent error. This optimal condition could be used as a guide for maceration of cannabis to obtain the extract containing a high content of cannabidiol and Δ9- tetrahydrocannabinol.


Assuntos
Canabidiol/análise , Cannabis/química , Dronabinol/isolamento & purificação , Extratos Vegetais/análise , Cromatografia Líquida de Alta Pressão , Dronabinol/análise , Métodos , Temperatura , Fatores de Tempo
5.
Forensic Sci Int ; 304: 109951, 2019 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-31563559

RESUMO

Hair analysis for the assessment of cannabis active use from passive consumption may be failed when performed by the sole detection of compounds present in plant material as well as in cannabis smoke like Δ-9-tetrahydrocannabinol (THC), cannabidiol (CBD), and cannabinol (CBN). For this reason, the determination of 11-nor-9-carboxy-Δ-9-tetrahydrocannabinol (THC-COOH) has been proposed by the Society of Hair Testing (SoHT) in order to prove active cannabis consumption. The identification of THC-COOH in hair will continue to be complicated by its acidic nature and the critical low concentration due to the preferential incorporation of basic compounds into hair shaft. Alternatively, 11-OH-THC may be considered as a complementary marker for THC administration. Our recent study reported an accurate validated procedure for THC, CBD, CBN and 11-OH-THC in hair, based on a GC/MS-MS method in electron ionization mode. However, unlike THC-COOH, a cut-off level for 11-OH-THC in hair has not been fixed yet. For this reason, the aim of this study is to propose a concentration value for 11-OH-THC in hair analysis in order to discriminate between chronic use and external contamination. Receiver operating characteristics (ROC) analysis was applied for cut-off evaluation after 11-OH-THC quantification in a pool of 672 THC-positive hair samples. Results have shown a concentration range between 0.01-5.34 ng/mg for THC (mean 0.34 ng/mg, median 0.12), 0.00-19.2 pg/mg for THC-COOH (mean 0.72 pg/mg, median 0.19 pg/mg) and 0.01-13.33 ng/mg for 11-OH-THC (mean 1.09 ng/mg, median 0.51 ng/mg) for scalp hair and between 0.03-6.32 ng/mg for THC (mean 0.82 ng/mg, median 0.30), 0.00-42.1 pg/mg for THC-COOH (mean 2.70 pg/mg, median 1.08 pg/mg) and 0.00-7.88 ng/mg for 11-OH-THC (mean 1.70 ng/mg, median 0.89 ng/mg) for body hair. Considering these experimental data collected in our laboratory, we propose a cut-off level of 0.5 for scalp and body hair, as indicative of cannabis active consumption. The ROC curve AUCs for 11-OH-THC were 0.873 and 0.884 in 590 scalp hair and 82 body hair samples, respectively. The comparison of the results for THC-COOH (control method) and 11-OH-THC (test method) was also made by means of the Cohen's kappa statistics providing a good agreement according to both Landis & Koch and Fleiss scales. Additionally, we suggest that the detection of both THC-COOH and 11-OH-THC should be mandatory in order to prove active intake and exclude false positive results from external contamination.


Assuntos
Dronabinol/análogos & derivados , Toxicologia Forense/normas , Cabelo/química , Alucinógenos/análise , Abuso de Maconha/diagnóstico , Biomarcadores/análise , Dronabinol/análise , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Valores de Referência
6.
J Mass Spectrom ; 54(10): 834-842, 2019 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-31498519

RESUMO

Recently in Canada and some states of the United States, marijuana (cannabis) has become fully legalized and regulated, for both medical and recreational purposes. This fact is going to make cannabis products such as edibles even more popular than ever before. Therefore, it is assumed that there will be a high demand for analytical methods, which are accurate and sensitive enough to be used in different forensic and pharmaceutical cannabis-related applications. Cannabis derivatives have an extreme range and number of constituents with possible interactions with one another. Thus, this characteristic leads to their vast and highly complex chemistry, which requires robust analytical tools to be able to precisely and accurately quantify and qualify them. We developed and validated an analytical method using desorption electrospray ionization (DESI)-mass spectrometry (MS) to accurately detect, characterize, and quantify cannabinoids and also offer an easy, cost-effective, and reliable technique, which can be performed in a short time for infused edibles in complex matrices such as chocolate. We evaluated a quantitative analysis of tetrahydrocannabinol (THC) in cannabis-infused chocolate with thin-layer chromatography (TLC)-DESI-MS and QuEChERS extraction method. Both techniques of TLC and QuEChERS are cost-effective and can be run in short time.


Assuntos
Cannabis/química , Chocolate/análise , Dronabinol/análise , Cromatografia em Camada Delgada/métodos , Dronabinol/análogos & derivados , Humanos , Limite de Detecção , Espectrometria de Massas por Ionização por Electrospray , Detecção do Abuso de Substâncias
7.
Drug Test Anal ; 11(10): 1486-1497, 2019 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-31442003

RESUMO

Point-of-collection testing (POCT) for Δ9 -tetrahydrocannabinol (THC) in oral fluid is increasingly used to detect driving under the influence of cannabis (DUIC). However, previous studies have questioned the reliability and accuracy of two commonly used POCT devices, the Securetec DrugWipe® 5 s (DW5s) and Dräger DrugTest® 5000 (DT5000). In the current placebo controlled, double-blind, crossover study we used liquid chromatography-tandem mass spectrometry (LC-MS/MS) to accurately quantify cannabinoid concentrations in the oral fluid of 14 participants at various timepoints (10, 60, 120, and 180 minutes) following vaporization of 125 mg of THC-dominant (11% THC; <1% CBD), THC/CBD equivalent (11% THC; 11% CBD) and placebo (<1% THC; <1% CBD) cannabis. At each timepoint, oral fluid was also screened using the DW5s (10 ng/mL THC cut-off) and DT5000 (10 ng/mL THC cut-off). LC-MS/MS analysis showed peak oral fluid THC concentrations at the 10 minute timepoint with a rapid decline thereafter. This trajectory did not differ with THC dominant and THC/CBD equivalent cannabis. With a 10 ng/mL confirmatory cut-off, 5% of DW5s test results were false positives and 16% false negatives. For the DT5000, 10% of test results were false positives and 9% false negatives. Neither the DW5s nor the DT5000 demonstrated the recommended >80% sensitivity, specificity and accuracy. Accuracy was lowest at 60 minutes, when THC concentrations were often close to the screening cut-off (10 ng/mL). POCT devices can be useful tools in detecting recent cannabis use; however, limitations should be noted, and confirmatory LC-MS/MS quantification of results is strongly advisable.


Assuntos
Dronabinol/análise , Psicotrópicos/análise , Saliva/química , Detecção do Abuso de Substâncias/métodos , Adulto , Canabidiol/análise , Cannabis/química , Estudos Cross-Over , Método Duplo-Cego , Feminino , Humanos , Masculino , Fumar Maconha , Reprodutibilidade dos Testes , Manejo de Espécimes/métodos , Espectrometria de Massas em Tandem/métodos , Volatilização , Adulto Jovem
8.
ACS Appl Mater Interfaces ; 11(38): 34777-34786, 2019 Sep 25.
Artigo em Inglês | MEDLINE | ID: mdl-31452365

RESUMO

Δ9-Tetrahydrocannabinol (THC) is the principal psychoactive component of cannabis, and there is an urgent need to build low-cost and portable devices that can detect its presence from breath. Similarly to alcohol detectors, these tools can be used by law enforcement to determine driver intoxication and enforce safer and more regulated use of cannabis. In this work, we propose to use a class of microporous crystals, metal-organic frameworks (MOFs), to selectively adsorb THC that can be later detected using optical, electrochemical, or fluorescence-based sensing methods. We computationally screened more than 5000 MOFs, highlighting the materials that have the largest affinity with THC, as well as the highest selectivity against water, showing that it is thermodynamically feasible for MOFs to adsorb THC from humid breath. We propose and compare different models for THC and different computational protocols to rank the promising materials, also presenting a novel approach to assess the permeability of a porous framework to nonspherical molecules. We identified three adsorption motifs in MOFs with high affinity to THC, which we refer to as "narrow channels", "thick walls", and "parking spots". Therefore, we expect our protocols and our findings to be generalizable for different classes of microporous materials and also for investigating the adsorption properties of other large molecules that, like THC, have a nonspherical shape.


Assuntos
Simulação por Computador , Dronabinol/análise , Estruturas Metalorgânicas/química , Modelos Químicos , Testes Respiratórios , Humanos
9.
Salud Publica Mex ; 61(4): 461-469, 2019.
Artigo em Espanhol | MEDLINE | ID: mdl-31314209

RESUMO

OBJECTIVE: Monitor drug use through wastewater metabolite measurement. MATERIALS AND METHODS: Wastewater samples were obtained from 31 wastewater treatment plants and 95 sites with specific populations (38 schools, 42 units of addiction treatment and 15 penitentiaries). Using ultra high liquid chromatography, we measured nine metabolites from six drugs. RESULTS: Eight out of nine drug metabolites were identified in the samples. Marijuana (THC-COOH), cocaine (benzoylecgonine) and methamphetamine were identified in schools, centers of addiction treatment and penitentiaries. Nuevo Laredo, Culiacan and Torreon had the highest consumption of cocaine, marijuana, amphetamine and methamphetamine. CONCLUSIONS: Monitoring drug use through wastewater is feasible in Mexico and could constitute a surveillance system to identify changes in the time.


Assuntos
/análise , Detecção do Abuso de Substâncias/métodos , Transtornos Relacionados ao Uso de Substâncias/epidemiologia , Águas Residuárias/química , Cannabis/química , Cromatografia Líquida de Alta Pressão , Cidades/epidemiologia , Cocaína/análogos & derivados , Cocaína/análise , Serviços de Saúde Comunitária/estatística & dados numéricos , Dronabinol/análogos & derivados , Dronabinol/análise , Estudos de Viabilidade , Heroína/análise , Humanos , Metanfetamina/análise , México/epidemiologia , Morfina/análise , N-Metil-3,4-Metilenodioxianfetamina/análise , Projetos Piloto , Instituições Acadêmicas/estatística & dados numéricos , Centros de Tratamento de Abuso de Substâncias/estatística & dados numéricos , Fatores de Tempo , Purificação da Água
10.
Analyst ; 144(16): 4952-4961, 2019 Aug 05.
Artigo em Inglês | MEDLINE | ID: mdl-31318364

RESUMO

Herein, we report the antioxidant activity of cannabidiol (CBD) and Δ9-tetrahydrocannabinol (THC) in pure and mixed solutions at different ratios, as well as of six different Cannabis sativa extracts containing various proportions of CBD and THC by using spectrophotometric (reducing power assay, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS), 2,2-diphenyl-1-picrylhydrazyl (DPPH), hypochlorous acid (HOCl) scavenging assays) and electrochemical methods (cyclic voltammetry and differential pulse voltammetry). The isolated cannabinoids, the different stoichiometric ratios of CBD and THC, and the natural extracts proved to have remarkable antioxidant properties in all the methods employed in this work. The antioxidant activity of CBD and THC was compared against that of the well-defined antioxidants such as ascorbic acid (AA), resveratrol (Resv) and (-)-epigallocatechin-3-gallate (EGCG). Clear evidence of the synergistic and antagonistic effects between CBD and THC regarding to their antioxidant activities was observed. Moreover, a good correlation was obtained between the optical and electrochemical methods, which proved that the reported experimental procedures can easily be adapted to determine the antioxidant activity of extracts from various Cannabis sativa species and related compounds.


Assuntos
Canabidiol/química , Cannabis/química , Dronabinol/química , Depuradores de Radicais Livres/química , Extratos Vegetais/química , Canabidiol/análise , Dronabinol/análise , Técnicas Eletroquímicas/métodos , Depuradores de Radicais Livres/análise , Extratos Vegetais/análise
11.
BMC Complement Altern Med ; 19(1): 132, 2019 Jun 17.
Artigo em Inglês | MEDLINE | ID: mdl-31208410

RESUMO

BACKGROUND: Nigerian Cannabis sativa (hemp) causes male gonadotoxicity by inducing hyperprolactinemia, down-regulation of hypothalamic-pituitary-testicular axis, and oxidative stress. Benin republic hemp has been preferred by illicit users in Nigeria but its effect on male fertility is not understood. This study determined and compared the compositions of Benin republic hemp ethanol extract (BHE) and Nigerian hemp. The effects of BHE on semen parameters, reproductive hormones, and anti-oxidant status, and the possibility of bromocriptine (prolactin inhibitor) to abolish hemp-induced toxicities in rats were also investigated. METHODS: Thirty-six male Wistar rats were blindly randomized into 6 oral treatment groups (n = 6 each). Groups I (control) and II received normal saline and bromocriptine (3 mg/kg) respectively. Groups III and IV received 2 mg/kg of BHE alone and in combination with bromocriptine respectively, while groups V and VI received 10 mg/kg BHE alone and in combination with bromocriptine respectively. Comparisons among the groups were done by one-way analysis of variance, followed by post-hoc Tukey multiple comparison test. Statistical significance was considered at p < 0.05. RESULTS: The BHE has no cannabichromene and tetrahydrocannabinol but a very small quantity of cannabinol and higher quantity of fatty acids when compared to Nigerian hemp. Both doses of BHE increased sperm count, morphology and viability but not motility. Co-administration of BHE with bromocriptine lowered sperm count but increased sperm morphology and viability. Bromocriptine and/or BHE caused reduction in the plasma prolactin level, increase in the plasma superoxide dismutase activity, but no significant change in the plasma gonadotropin releasing hormone, follicle stimulating hormone (except for the increase in rats that received bromocriptine+ 10 mg/kg BHE), luteinizing hormone, estradiol, malondialdehyde and glutathione peroxidase. The 10 mg/kg BHE or bromocriptine+BHE (both doses) increased total anti-oxidant capacity and catalase. CONCLUSIONS: The BHE improves semen parameters by reducing plasma prolactin and enhancing plasma anti-oxidant status. Its pro-fertility potential might be associated with its deficiency in the widely known gonadotoxic phytocannabinoids.


Assuntos
Antioxidantes/metabolismo , Canabinoides/análise , Cannabis/química , Dronabinol/análise , Fármacos para a Fertilidade Masculina/farmacologia , Extratos Vegetais/farmacologia , Prolactina/metabolismo , Sêmen/efeitos dos fármacos , Animais , Canabinoides/farmacologia , Dronabinol/farmacologia , Fertilidade/efeitos dos fármacos , Fármacos para a Fertilidade Masculina/análise , Masculino , Extratos Vegetais/análise , Ratos , Sêmen/metabolismo
12.
Planta Med ; 85(9-10): 781-796, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-31096276

RESUMO

The phytochemical diversity of Cannabis chemovars is not well understood, and many chemovars were created in informal breeding programs without records of parentage or the criteria for selection. Key criteria for selection sometimes included aroma notes and visual cues, which some breeders associated with pharmacological activity. We hypothesized that the process of selection for scents believed to be related to specific tetrahydrocannabinol levels has resulted in modified terpene biosynthesis in these chemovars. Thirty-two cannabinoids, 29 monoterpenes and 38 sesquiterpenes were measured in 33 chemovars from 5 licensed producers. A classification system based on cannabinoid content was used with targeted metabolomic tools to determine relationships in the phytochemistry. Three monoterpenes, limonene, ß-myrcene, and α-pinene, and two sesquiterpenes, caryophyllene and humulene, were abundant in the majority of chemovars. Nine terpenes were present in tetrahydrocannabinol-dominant chemovars. Three monoterpenes and four sesquiterpenes were predominantly found in cannabidiol-containing chemovars. Low abundance terpenes may have been the aromatic cues identified by breeders. The medicinal activity of some of the terpenes is likely to contribute to the pharmacological effect of specific chemovars. Together, these data demonstrate the synergy of compounds in Cannabis chemovars and point to the need for additional research to understand the phytochemical complexity.


Assuntos
Canabinoides/análise , Cannabis/química , Cannabis/metabolismo , Odorantes/análise , Terpenos/análise , Canabidiol/análise , Canabinoides/metabolismo , Cannabis/classificação , Dronabinol/análise , Metabolômica/métodos , Melhoramento Vegetal , Terpenos/metabolismo
13.
Yakugaku Zasshi ; 139(5): 693-697, 2019.
Artigo em Japonês | MEDLINE | ID: mdl-31061337

RESUMO

The number of persons arrested in Japan for drug-related offenses in 2016 increased from the previous year. Especially, cannabis offenses have increased since 2014, with more than 2000 persons arrested in 2015. As a feature of the year 2017, we analyzed many cannabis concentrates, called "Cannabis wax", in the process of analyzing cannabis in the Narcotics Control Department. "Cannabis wax" refers to concentrates of the hallucinogenic component of cannabis, tetrahydrocannabinol (THC). Increasingly, cannabis wax containing 50 times higher THC than general dry cannabis has been confiscated. More than 2300 compounds are currently regulated as new psychoactive substances in Japan. In a recent trend, there is an increasing number of cases in which a wide range of regulated substances have been seized and confiscated, ranging from those that have been abused for a long time, to those that are newly regulated. Many structural isomers are present among these, and we are constantly developing techniques for the rapid and accurate analysis of these compounds.


Assuntos
Crime/estatística & dados numéricos , Dronabinol/análise , Transtornos Relacionados ao Uso de Substâncias/epidemiologia , Cromatografia , Humanos , Isomerismo , Japão/epidemiologia , Abuso de Maconha/epidemiologia , Abuso de Maconha/prevenção & controle , Espectrometria de Massas , Entorpecentes/análise , Transtornos Relacionados ao Uso de Substâncias/prevenção & controle
15.
Forensic Sci Int ; 299: 142-150, 2019 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-31005710

RESUMO

Analysis of cannabis has gained new importance worldwide, mainly for quality control within the legalized recreational and medical cannabis industry, but also for forensic differentiation between drug-type cannabis and legal products such as fiber hemp and CBD-rich/THC-poor cannabis. We herein present an HPLC-DAD method for quantitative analysis of major neutral and acidic cannabinoids in herbal cannabis and hashish: Δ9-tetrahydrocannabinol (THC), Δ9-tetrahydrocannabinolic acid A (THCA), cannabidiol (CBD), cannabidiolic acid (CBDA), and cannabinol (CBN). Plant material was dried, homogenized and extracted with a mixture of methanol/hexane. Chromatographic separation of the analytes was achieved on a core-shell C8 column using gradient elution with water/acetonitrile containing 0.1% formic acid. The analytical run time was 13 min and analytes were detected at 210 nm. The method is selective, sensitive, accurate, and precise, as confirmed through validation according to ICH and AOAC guidelines. Linearity in herbal cannabis ranged from 0.04 to 4.00% for the neutral cannabinoids, and from 0.40 to 20% for the acids. Linear ranges in hashish samples were 0.13-13.33% and 1.33-66.66%, respectively. The presented method was successfully applied to characterize 110 cannabis samples seized by the Swiss police, demonstrating its applicability for routine cannabis potency testing in the forensic setting.


Assuntos
Cannabis/química , Cromatografia Líquida de Alta Pressão/métodos , Canabinoides/análise , Canabinol/análise , Dronabinol/análise , Limite de Detecção
16.
J Sep Sci ; 42(11): 1972-1979, 2019 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-30919567

RESUMO

Three silica hydride based novel chromatographic phases chemically-bonded with allyloxy-DL-alpha-tocopherol, allylpentafluorophenyl, and 1-eicosene moieties were evaluated as separation media for selected phytocannabinoids and other substances of abuse. In order to assess column selectivity, a series of reference standards was analyzed and detected by using liquid chromatography with mass spectrometry. Further, quantitative detections of cannabidiol and tetrahydrocannabinol were attempted for the extracts of cannabis plants and cannabidiol gummy formulation. For potential bioanalytical applications, the columns were evaluated for substance screening in a human urine matrix. In summary, the newly developed columns are functional and effective for the analysis of phytocannabinoids and various psychoactive drugs with or without the presence of biological matrices.


Assuntos
Canabinoides/análise , Canabinoides/urina , Cromatografia Líquida de Alta Pressão/métodos , Extratos Vegetais/análise , Psicotrópicos/análise , Psicotrópicos/urina , Silicatos/química , Cromatografia Líquida de Alta Pressão/instrumentação , Dronabinol/análise , Dronabinol/urina , Humanos , Extratos Vegetais/urina
17.
J Chromatogr A ; 1597: 109-118, 2019 Jul 19.
Artigo em Inglês | MEDLINE | ID: mdl-30910385

RESUMO

An azo coupling-based derivatization method is reported for high-sensitivity liquid chromatography-tandem mass spectrometry (LC-MS/MS) quantitation of tetrahydrocannabinol (THC) and other aromatic compounds, i.e. phenols and amines. Through the azo coupling of a diazonium to an analyte, it produces a derivatized analyte which has enhanced ionization efficiency and results in high-response fragments in tandem mass spectrometry. The derivatization method was applied to six typical aromatic compounds using three different diazonium salts as derivatization reagents, demonstrating its applicability to a variety of analytes and reagents. The derivatization reaction can be directly carried out in neat samples, and after derivatization the samples can be immediately sent to the LC-MS/MS instrument for analysis. These advantages facilitate a one-step sample preparation procedure that can be completed in less than one hour, allowing for a "derivatize & shoot" lab workflow. The derivatization method was applied to establish an LC-MS/MS assay for the quantitation of THC in human breath samples. The derivatization conditions were studied in this application, including the effects of acidity, organic solvent, and diazonium concentration in the reaction. The THC derivatization assay was validated and achieved a limit of quantitation (LOQ) of 0.50 pg/ml using either of the two regio-isomers of the azo-derivative of THC (THC-DRV). To prove that the derivatization method has compatibility with complex-matrix samples, a THC derivatization assay for serum samples was established, in which the azo coupling reaction was directly carried out in crude protein-precipitated supernatants. An LOQ of 5.0 pg/ml was achieved. In addition, excellent correlation between THC derivatization and non-derivatization assays was found in the analysis of whole blood samples.


Assuntos
Testes Respiratórios/métodos , Cromatografia Líquida , Dronabinol/análise , Espectrometria de Massas em Tandem , Aminas/análise , Análise Química do Sangue , Dronabinol/sangue , Humanos , Indicadores e Reagentes , Limite de Detecção , Fenóis/análise
19.
Forensic Sci Int ; 295: 219-225, 2019 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-30600116

RESUMO

Cannabis is the second most commonly abused illicit drug after methamphetamine in South Korea. To prove cannabis consumption, 11-nor-9-carboxy-tetrahydrocannabinol (THC-COOH), the metabolite of tetrahydrocannabinol (THC), was screened for in a hair analysis. In this study, we developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis method, which was used to analyze authentic hair samples in 2017. Possible contaminants on the surface of hair samples were eliminated by washing twice each with 2mL of methanol and distilled water. After adding an internal standard (THC-COOH-d3), the hair samples (about 20mg each) were digested with 1M NaOH, extracted twice with mixed organic solvents (n-hexane:ethyl acetate), and analyzed by an LC-MS/MS system. Identification and quantification of THC-COOH and THC-COOH-d3 were performed using a multiple reaction monitoring (MRM) mode at m/z 245 and 191 and m/z 248, respectively (quantifier ions are underlined). The following validation parameters were evaluated: selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, matrix effect, and recovery. The LOD and LOQ of the method was 0.1pg/mg. Good linearity was achieved for THC-COOH in the range from 0.1 to 20pg/mg. The method showed an acceptable precision and accuracy, both of which were less than 15% at the three concentrations of THC-COOH (0.2, 1, and 10pg/mg). THC-COOH showed ion suppression at these three concentrations. The concentrations of THC-COOH in the authentic hair samples ranged from 0.10 to 27.30pg/mg (total 586 cases), and its concentrations were classified as low, medium, or high ranges, i.e., 0.10-0.39pg/mg, 0.39-1.99pg/mg, or 1.99-27.30pg/mg, respectively, according to statistical evaluation. This method showed the possibility of replacing the existing gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. However, further development of our LC-MS/MS method is necessary in order to meet the recommended 0.05pg/mg cut-off.


Assuntos
Dronabinol/análogos & derivados , Usuários de Drogas , Cabelo/química , Detecção do Abuso de Substâncias , Adolescente , Adulto , Idoso , Cromatografia Líquida , Dronabinol/análise , Feminino , Toxicologia Forense , Humanos , Limite de Detecção , Masculino , Pessoa de Meia-Idade , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem , Adulto Jovem
20.
Eur Arch Psychiatry Clin Neurosci ; 269(1): 5-15, 2019 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-30671616

RESUMO

Through the potency monitoring program at the University of Mississippi supported by National Institute on Drug Abuse (NIDA), a total of 18108 samples of cannabis preparations have been analyzed over the last decade, using a validated GC/FID method. The samples are classified as sinsemilla, marijuana, ditchweed, hashish, and hash oil (now referred to as cannabis concentrate). The number of samples received over the last 5 years has decreased dramatically due to the legalization of marijuana either for medical or for recreational purposes in many US states. The results showed that the mean Δ9-THC concentration has increased dramatically over the last 10 years, from 8.9% in 2008 to 17.1% in 2017. The mean Δ9-THC:CBD ratio also rose substantially from 23 in 2008 to 104 in 2017. There was also marked increase in the proportion of hash oil samples (concentrates) seized (0.5-4.7%) and their mean Δ9-THC concentration (6.7-55.7%) from 2008 to 2017. Other potency monitoring programs are also present in several European countries such as The Netherlands, United Kingdom, France, and Italy. These programs have also documented increases in Δ9-THC concentrations and Δ9-THC:CBD ratios in cannabis. These trends in the last decade suggest that cannabis is becoming an increasingly harmful product in the USA and Europe.


Assuntos
Agonistas de Receptores de Canabinoides , Cannabis/química , Dronabinol , Monitoramento de Medicamentos , Agonistas de Receptores de Canabinoides/análise , Cannabis/classificação , Cromatografia Gasosa , Dronabinol/análise , Europa (Continente) , Humanos , /química , Estados Unidos
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