RESUMO
We report the synthesis, characterization, and application of [Zn(1,4-benzenedicarboxylate)(H2 O)2 ]n , Zn(1,4-benzenedicarboxylate)0.99 (NH2 -1,4-benzenedicarboxylate)0.01 (H2 O)2 ]n , [Zn(1,4-benzenedicarboxylate)0.95 (NH2 -1,4-benzenedicarboxylate)0.05 (H2 O)2 ]n , and [Zn(1,4-benzenedicarboxylate)0.9 (NH2 -1,4-benzenedicarboxylate)0.1 (H2 O)2 ]n as sorbents for the extraction of multiclass pesticides from coconut palm. Liquid chromatography with ultraviolet diode array detection was used as the analysis technique, and the experiments were performed at one fortification level (0.1 µg/g). The recoveries were 47-67, 51-70, 58-72, and 64-76% for [Zn(1,4-benzenedicarboxylate)(H2 O)2 ]n , Zn(1,4-benzenedicarboxylate)0.99 (NH2 -1,4-benzenedicarboxylate)0.01 (H2 O)2 ]n , [Zn(1,4-benzenedicarboxylate)0.95 (NH2 -1,4-benzenedicarboxylate)0.05 (H2 O)2 ]n , and [Zn(1,4-benzenelate)0.95 (NH2 -1,4-benzenedicarboxylate)0.05 (H2 O)2 ]n , and [Zn(1,4-benzenedicarboxylate)0.9 (NH2 -1,4-benzenedicarboxylate)0.1 (H2 O)2 ]n , respectively, with relative standard deviation ranging from 1 to 7% (n = 3). Detection and quantification limits were 0.01-0.05 and 0.05-0.2 µg/g, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.01-10.0 µg/g) with r2 > 0.9991. A direct comparison of [Zn(1,4-benzenedicarboxylate)0.9 (NH2 -1,4-benzenedicarboxylate)0.1 (H2 O)2 ]n with the commercially available neutral alumina showed that [Zn(1,4-benzenedicarboxylate)0.9 (NH2 -1,4-benzenedicarboxylate)0.1 (H2 O)2 ]n was a similar extracting phase for the pesticides investigated.
Assuntos
Cocos/química , Estruturas Metalorgânicas , Praguicidas/análise , Cromatografia Líquida , Extração em Fase SólidaRESUMO
A method was developed using matrix solid-phase dispersion, together with liquid chromatography with ultraviolet diode array detector for determination of carbofuran, difenoconazole, ß-cyfluthrin, spirodiclofen and thiophanate-methyl in stem of coconut palm. The best results were obtained using 2.0 g of stem, 1.6 g of Florisil as sorbent and cyclohexane:acetone mixture (4:1). The method was validated using stem samples spiked with pesticides at four concentration levels (0.05-2.0 µg/g). Average recoveries ranged from 70 % to 114.3 %, with relative standard deviations between 1.2 % and 19.2 %. Detection and quantification limits were in the ranges 0.02-0.03 and 0.05-0.1 µg/g, respectively.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Cocos/química , Resíduos de Praguicidas/análise , Caules de Planta/química , Extração em Fase Sólida/métodos , 4-Butirolactona/análogos & derivados , 4-Butirolactona/análise , Acetona/química , Carbofurano/análise , Cicloexanos/química , Dioxolanos/análise , Silicatos de Magnésio/química , Nitrilas/análise , Piretrinas/análise , Reprodutibilidade dos Testes , Compostos de Espiro/análise , Tiofanato/análise , Triazóis/análiseRESUMO
Metal-organic frameworks aluminum terephthalate MIL-53 and Cu-benzene-1,3,5-tricarboxylate (BTC) were tested for extraction of pyrimethanil, ametryn, dichlofluanid, tetraconazole, flumetralin, kresoximmethyl, and tebuconazole from the medicinal plant Hyptis pectinata, with analysis using GC/MS in the selected ion monitoring mode. Experiments carried out at different fortification levels (0.1, 0.5, and 1.0 microg/g) resulted in recoveries in the range 61 to 107% with RSD values between 3 and 12% for the metal-organic framework materials. Detection and quantification limits ranged from 0.02 to 0.07 and 0.05 to 0.1 microg/g, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.04-20.0 microg/g), with correlation coefficients ranging from 0.9987 to 0.9998. Comparison of MIL-53 and Cu-BTC with C18-bonded silica showed good performance of the MIL-53 metal-organic framework as a sorbent for the pesticides tested.
Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Hyptis/química , Metais/química , Praguicidas/química , Extração em Fase Sólida/métodos , Adsorção , Resíduos de Praguicidas/química , Plantas Medicinais/químicaRESUMO
Alkaloids play an important role in the chemical composition of tobacco, due to their effects that have led to the global consumption of this commodity. The ß-carboline alkaloids present inhibitory action against the enzyme monoamine oxidase (MAO), which enhances the susceptibility to chemical dependence in smokers. There is a need for scientific studies to ensure the correct identification and quantification of these compounds in tobacco matrices. In this work, we present the development and validation of a microextraction analytical method for determination and quantification of the alkaloids harmaline, harmalol, harmane, harmine, norharmane, and tetrahydroharmine in natural and processed samples of tobacco, employing micro-matrix solid-phase dispersion (µMSPD), ultra-performance liquid chromatography (UPLC), and mass spectrometry (MS). The optimized µMSPD procedure employed of 0.01 g of sample, 0.1 g of Discovery® DPA-6S adsorbent, and elution with 2 mL of aqueous 1 % formic acid solution, resulting in a fast, practical, economical, and environmentally friendly technique. Validation of the methodology showed that it presented good linearity (R2 > 0.9945), satisfactory accuracy and precision (in the range from 72 ± 16 % to 109 ± 9 %), and limits of quantification (LOQ) and detection (LOD) in the ranges 0.02-1.0 µg g-1 and 0.01-0.2 µg g-1, respectively. The developed method was applied to tobacco samples, proving to be efficient for determination of ß-carboline alkaloids. The compounds harmane and norharmane were quantified in samples of fresh tobacco leaves, cured tobacco leaves, twisted tobacco, and cigarettes. Harmine was only not quantified in the cigarettes.
Assuntos
Alcaloides , Produtos do Tabaco , Alcaloides/análise , Carbolinas/química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida , Harmina/análise , Harmina/química , Espectrometria de Massas , Nicotiana , Produtos do Tabaco/análiseRESUMO
The metal-organic framework (∞)[(La(0.9)Eu(0.1))(2)(DPA)(3)(H(2)O)(3)] was tested for extraction of pyrimicarb, procymidone, malathion, methyl parathion and α- and ß-endosulfan from lettuce, with analysis using GC/MS in SIM mode. Experiments were carried out in triplicate at two fortification levels (0.1 and 0.5 mg/kg), and resulted in recoveries in the range of 78-107%, with RSD values between 1.6 and 8.0% for (∞)[(La(0.9)Eu(0.1))(2)(DPA)(3)(H(2)O)(3)] sorbent. Detection and quantification limits ranged from 0.02 to 0.05 mg/kg and from 0.05 to 0.10 mg/kg, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.05-10.0 µg/mL), with correlation coefficients ranging from 0.9990 to 0.9997. Comparison between (∞)[(La(0.9)Eu(0.1))(2)(DPA)(3)(H(2)O)(3)] and conventional sorbent (silica gel) showed better performance of the (∞)[(La(0.9)Eu(0.1))(2)(DPA)(3)(H(2)O)(3)] polymeric sorbent for all pesticides tested.
Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Lactuca/química , Praguicidas/análise , Extração em Fase Sólida/instrumentação , Limite de Detecção , Padrões de Referência , Reprodutibilidade dos Testes , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
An extraction method based on matrix solid-phase dispersion was developed to determine pirimicarb, methyl parathion, malathion, procymidone, alpha-endosulfan and beta-endosulfan in lettuce using gas chromatography-mass spectrometry. The best results were obtained using 4.0 g of lettuce, 2.0 g of silica as dispersant sorbent, 0.1 g of activated carbon as clean up sorbent and acetonitrile as eluting solvent. The method was validated using lettuce samples fortified with pesticides at six different concentration levels (0.1 to 2.0 mg/kg). Average recoveries (7 replicates) ranged from 50 to 120%, with relative standard deviations between 0.6 and 8.0%. Detection and quantification limits for lettuce ranged from 0.01 to 0.02 mg/kg and 0.04 to 0.10 mg/kg, respectively.
Assuntos
Carbamatos/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Hidrocarbonetos Clorados/análise , Lactuca/química , Compostos Organofosforados/análise , Resíduos de Praguicidas/análise , Acetonitrilas/química , Compostos Bicíclicos com Pontes/análise , Endossulfano/análise , Malation/análise , Metil Paration/análise , Pirimidinas/análise , Extração em Fase Sólida/métodos , Solventes/químicaRESUMO
The 2D coordination polymer (infinity[Gd(DPA)(HDPA)]) was tested for extraction of acephate, chlorpropham, pirimicarb, bifenthrin, tetradifon, and phosalone from the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products, using GC/MS, SIM. Considering that there are no Brazilian regulations concerning maximum permissible pesticide residue concentrations in medicinal herbs, recovery experiments were carried out (seven replicates), at two arbitrary fortification levels (0.5 and 1.0 mg/kg), resulting in recoveries in range of 20 to 107.7% and SDRSDs were between 5.6 and 29.1% for infinity[Gd(DPA)(HDPA)] sorbent. Detection and quantification limits for herb ranged from 0.10 to 0.15 mg/kg and from 0.15 to 0.25 mg/kg, respectively, for the different pesticides studied. The developed method is linear over the range assayed, 0.5-10.0 microg/mL, with correlation coefficients ranging from 0.9975 to 0.9986 for all pesticides. Comparison between infinity[Gd(DPA)(HDPA)] sorbent and conventional sorbent (neutral alumina) showed similar performance of infinity[Gd(DPA)(HDPA)] polymeric sorbent for three (bifenthrin, tetradifon, and phosalone) out of six pesticides tested.
Assuntos
Cordia/química , Cromatografia Gasosa-Espectrometria de Massas , Resíduos de Praguicidas/análise , Polímeros/química , Extração em Fase Sólida , Adsorção , Brasil , Gadolínio/química , Cromatografia Gasosa-Espectrometria de Massas/instrumentação , Cromatografia Gasosa-Espectrometria de Massas/métodos , Humanos , Plantas Medicinais/química , Extração em Fase Sólida/instrumentação , Extração em Fase Sólida/métodosRESUMO
A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selected-ion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexane-dichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9%, with relative standard deviations between 6.3 and 26%. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.
Assuntos
Cordia/química , Resíduos de Praguicidas/análise , Praguicidas/análise , Brasil , Cromatografia Gasosa-Espectrometria de Massas , Folhas de Planta/química , Padrões de Referência , Reprodutibilidade dos Testes , SolventesRESUMO
Background: Pesticides are applied for pest control during the production of cereal grains used in beer production. Given the risks for consumers, it is important to analyze the pesticide residues. Objective: Quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based methods are very effective, and improvement in the cleanup step is an important approach. Methods: Primary secondary amine (PSA) and magnesium silicate were evaluated for dispersive-solid-phase extraction (d-SPE) cleanup step in extracts provided by the QuEChERS method in combination with GC-tandem MS for the determination of acetamiprid, terburfos, alachlor, ametryn, atrazine, azoxystrobin, carbofuran, carbosulfan, cypermethrin, deltamethrin, difenoconazole, esfenvalerate, flutriafol, thiamethoxam, and parathion-methyl in lager beer. Results: The amount of 50 mg of magnesium silicate was suitable for cleaning up beer extract as an alternative d-SPE material to PSA. The method was validated using beer fortified with pesticides at three concentration levels (0.002, 0.01, and 0.1 µg/mL). Average recoveries ranged from 70 to 123%, with RSDs between 0.3 and 10.5 %. Matrix effects were observed by comparing the slope of matrix-matched standard calibration with that of solvent. The method provided good linearity at the concentration levels of 0.001-2.5 µg/mL. Detection limits ranged from 0.0001 to 0.0007 µg/mL and quantification limits ranged from 0.001 to 0.006 µg/mL. The method was applied to nine beer brands. Conclusions: Results showed that magnesium silicate is an efficient alternative cleanup material to reduce analysis costs while maintaining the method reliability and accuracy. Highlights: Magnesium silicate was effective as adsorbent for d-SPE step in the analysis of pesticides in beer.
Assuntos
Cerveja/análise , Silicatos de Magnésio/química , Praguicidas/isolamento & purificação , Extração em Fase Sólida , Adsorção , Cromatografia Gasosa , Espectrometria de Massas em TandemRESUMO
A method based on solid-phase microextraction (SPME) and gas chromatography with flame ionization detection (GC-FID) has been optimized for the determination of benzene, toluene, ethylbenzene and xylenes (BTEX) in water released from a waste treatment plant. The extraction step was optimized using fractional factorial and central composite designs including the following experimental factors: saline concentration; extraction time; desorption time; agitation velocity; headspace volume. A multiple function was used to describe the experimental conditions for simultaneous extraction of the compounds. The procedure, based on direct SPME at 50 degrees C, using a polydimethylsiloxane fiber, showed good linearity (r>0.997 over a concentration range 2-200 microg L(-1)) and repeatability (relative standard deviation (RSD)<4.23%) for all compounds, with limits of detection ranging from 0.05 to 0.28 microg L(-1), and limits of quantification ranging from 0.14 to 0.84 microg L(-1). Concentrations of the target compounds in these samples were between 145.8 and 1891 microg L(-1).
Assuntos
Derivados de Benzeno/análise , Benzeno/análise , Cromatografia Gasosa/métodos , Microextração em Fase Sólida/métodos , Tolueno/análise , Poluentes Químicos da Água/análise , Xilenos/análise , Análise Multivariada , Reprodutibilidade dos Testes , Incerteza , Eliminação de Resíduos LíquidosRESUMO
A simple and effective extraction method based on matrix solid-phase dispersion (MSPD) was developed to determine bifenthrin, buprofezin, tetradifon, and vinclozolin in propolis using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS, SIM). Different method conditions were evaluated, for example type of solid phase (C(18), alumina, silica, and Florisil), the amount of solid phase and eluent (n-hexane, dichloromethane, dichloromethane-n-hexane (8:2 and 1:1, v/v) and dichloromethane-ethyl acetate (9:1, 8:2 and 7:3, v/v)). The best results were obtained using 0.5 g propolis, 1.0 g silica as dispersant sorbent, 1.0 g Florisil as clean-up sorbent, and dichloromethane-ethyl acetate (9:1, v/v) as eluting solvent. The method was validated by analysis of propolis samples fortified at different concentration levels (0.25 to 1.0 mg kg(-1)). Average recoveries (four replicates) ranged from 67% to 175% with relative standard deviation between 5.6% and 12.1%. Detection and quantification limits ranged from 0.05 to 0.10 mg kg(-1) and 0.15 to 0.25 mg kg(-1) propolis, respectively.
Assuntos
Hidrocarbonetos Clorados/análise , Oxazóis/análise , Própole/análise , Piretrinas/análise , Tiadiazinas/análise , Calibragem , Cromatografia Gasosa-Espectrometria de Massas , Hidrocarbonetos Clorados/química , Estrutura Molecular , Oxazóis/química , Própole/química , Piretrinas/química , Tiadiazinas/químicaRESUMO
Background: A simple and effective extraction method based on ultrasonic solvent extraction and liquid-liquid microextraction (as the cleaning step) was developed to determine seven pesticide residues in roasted coffee (Coffea arabica) using ultra-performance LC-tandem MS. Objective: Different parameters of the method were evaluated, including solvent type and amount and sonication time. The best results were obtained using 1.0 g roasted coffee and acetonitrile (5 mL) as the extraction solvent with sonication for 15 min. The method was validated using roasted coffee samples fortified with pesticides at different concentration levels (0.1, 0.2, 0.3, and 0.5 µg/kg). Average recoveries (three replicates) ranged from 74.3 to 99.9%, with RSDs between 0.7 and 10.2%. Results: The method showed good linearity for all the pesticides studied, with correlation coefficients >0.99. The detection limits ranged from 0.02 to 0.05 µg/kg, and the quantification limit for all the compounds was 0.10 µg/kg. The proposed method was applied for analysis of the compounds in commercial coffee samples from a producer in Minas Gerais State, Brazil. No residues of the pesticides were detected in the samples. Highlights: Ultrasonic solvent extraction was effective in the analysis of pesticides in roasted coffee.
RESUMO
A method is optimized to determine benomyl (as carbendazim derivative) in shiitake mushrooms. It is based on the extraction of the fungicide with an ethyl acetate-hexane mixture and a further analysis of the extract by high-performance liquid chromatography-UV. Mean recoveries are evaluated and range from 76% to 86% with relative standard deviation between 1.1% and 5.8%. The limit of quantitation (0.5 mg/Kg) is lower than the maximum residue level established by European legislation. The method is successfully applied to the analysis of shiitake mushrooms cultivated on eucalyptus logs treated with Benlate 500 (benomyl as active ingredient) under natural environmental conditions.
Assuntos
Agaricales/química , Cromatografia Líquida/métodos , Espectrofotometria Ultravioleta/métodos , Aminoácidos/síntese química , Fluoresceína-5-Isotiocianato , Concentração de Íons de Hidrogênio , Estereoisomerismo , Tensoativos/químicaRESUMO
Ayahuasca is a potent hallucinogenic beverage prepared from Banisteriopsis caapi in combination with other psychoactive plants. N,N-dimethyltryptamine, tryptamine, harmine, harmaline, harmalol, and tetrahydroharmine were quantified in ayahuasca samples using a simple and low-cost method based on SPE and LC with UV diode-array detection. The experimental variables that affect the SPE method, such as type of solid phase and nature of solvent, were optimized. The method showed good linearity (r > 0.9902) and repeatability (RSD < 0.8%) for alkaloid compounds, with an LOD of 0.12 mg/L. The proposed method was used to analyze 20 samples from an ayahuasca cooking process from a religious group located in the municipality of Fortaleza, state of Ceará, Brazil. The results showed that concentrations of the target compounds ranged from 0.3 to 36.7 g/L for these samples.
Assuntos
Banisteriopsis/química , Bebidas/análise , Carbolinas/análise , Alucinógenos/análise , Triptaminas/análise , BrasilRESUMO
In this study, we describe the synthetic approach, crystallographic structure, luminescent behavior and elucidation of the channels of the energy conversion in heteronuclear coordination polymers with emission in the visible (Eu(3+) and organic ligand) and near-infrared (Nd(3+)) range. The [(Nd0.9Eu0.1)2(dipc)3(H2O)3]n·nH2O, [(Nd0.7Eu0.3)2(dipc)3(H2O)3]n·nH2O, [(Nd0.5Eu0.5)2(dipc)3(H2O)3]n·nH2O, [(Nd0.3Eu0.7)2(dipc)3(H2O)3]n·nH2O, [(Nd0.1Eu0.9)2(dipc)3(H2O)3]n·nH2O, [Eu2(dipc)3(H2O)3]n·nH2O and [Nd2(dipc)3(H2O)3]n·nH2O materials are obtained by hydrothermal conditions from pyridine-2,6-dicarboxylic acid (H2dipc) and Ln2O3 oxide (Ln = Eu and Nd). The fine structures in the emission spectrum and spectral profile are used to investigate the ion responsible for the emission characteristics of a material (6), based on coordination polyhedron. The heteronuclear systems show emission in the dual spectral range (NIR-VIS) tuned for blue or red. The tuning of emission on the red (Eu(3+)) or blue (organic ligand) range may be performed by controlling the stoichiometric ratio of the lanthanide ions and by controlling the excitation wavelength. Nd(3+) ions display self-absorption of emission to dipc ligand, resulting in interference on the emission band profile ranging from 400 to 600 nm. The energetic process of energy transfer is operated by a cascade of energy transfer, from dipc ligand mainly to Eu(3+) ions and finishing on the Nd(3+) ion. The efficient sensitization to Nd(3+) by Eu(3+) ions is due to the presence of many resonant energy levels and the short distance between these ions.
RESUMO
A simple method was developed for the determination of fluquinconazole, pyrimethanil, and clofentezine in whole fruit; peel; and pulp of mango, apple, and papaya. These compounds were extracted from fruit samples with a mixture of ethyl acetate-n-hexane (1 + 1, v/v). An aliquot (2 mL) of the extract was evaporated to near dryness under a stream of nitrogen, and the residue was dissolved with 2 mL methanol. The analysis was performed by means of liquid chromatography with ultraviolet detection at 254 nm using a gradient solvent system. The method was validated with fortified fruit samples at concentration levels of 0.05, 0.10, 0.20, and 0.50 mg/kg. Average recoveries (4-8 replicates) ranged from 80 to 95% with relative standard deviations between 3.5 and 12.7%. Detection limits ranged from 0.03 to 0.05 mg/kg for fruit pulp and 0.03 mg/kg for whole fruit. The quantitation limits ranged from 0.05 to 0.10 mg/kg for fruit pulp and 0.05 mg/kg for whole fruit. The analytical method was applied to fruit samples obtained from local markets.
Assuntos
Clorobenzenos/análise , Frutas/química , Fungicidas Industriais/análise , Pirimidinas/análise , Cromatografia Líquida , Reprodutibilidade dos TestesRESUMO
A novel analytical approach combining solid-phase microextraction (SPME)/gas chromatography ion trap mass spectrometry (GC-IT-MS) was developed for the detection and quantification N,N-dimethyltryptamine (DMT), a powerful psychoactive indole alkaloid present in a variety of South American indigenous beverages, such as ayahuasca and vinho da jurema. These particular plant products, often used within a religious context, are increasingly consumed throughout the world following an expansion of religious groups and the availability of plant material over the Internet and high street shops. The method described in the present study included the use of SPME in headspace mode combined GC-IT-MS and included the optimization of the SPME procedure using multivariate techniques. The method was performed with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in headspace mode (70 min at 60 °C) which resulted in good precision (RSD<8.6%) and accuracy values (71-109%). Detection and quantification limits obtained for DMT were 0.78 and 9.5 mg L(-1), respectively and good linearity (1.56-300 mg L(-1), r(2)=0.9975) was also observed. In addition, the proposed method showed good robustness and allowed for the minimization of sample manipulation. Five jurema beverage samples were prepared in the laboratory in order to study the impact of temperature, pH and ethanol on the ability to extract DMT into solution. The developed method was then applied to the analysis of twelve real ayahuasca and vinho da jurema samples, obtained from Brazilian religious groups, which revealed DMT concentration levels between 0.10 and 1.81 g L(-1).
Assuntos
Banisteriopsis/química , Bebidas/análise , Alucinógenos/análise , N,N-Dimetiltriptamina/análise , Extratos Vegetais/química , Psychotria/química , Comportamento Ritualístico , Dimetilpolisiloxanos , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Concentração de Íons de Hidrogênio , Limite de Detecção , Microextração em Fase Sólida , Temperatura , Compostos de VinilaRESUMO
The modification of MCM-41 was performed with 3-aminopropropyltrimethoxysilane. The structural order and textural properties of the synthesized materials were studied by X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetry/differential thermogravimetry, nitrogen adsorption, and desorption analysis. The adsorption capacity of NH2-MCM-41 was studied with Remazol Red dye. The following parameters were studied in the adsorption process: pH, temperature, adsorbent dosage, and initial concentration. The desorption process was studied in different concentrations of NaOH solutions. The Freundlich isotherm model was found to be fit with the equilibrium isotherm data. Kinetics of adsorption follows the modified Avrami rate equation. The maximum adsorption capacity was estimated to be 45.9 mg g(-1), with removal of the dye of 99.1%. The NH2-MCM-41 material exhibited high desorption capacity with 98.1%.
Assuntos
Corantes/isolamento & purificação , Dióxido de Silício/análise , Dióxido de Silício/química , Adsorção , Concentração de Íons de Hidrogênio , Cinética , Nitrogênio/análise , Nitrogênio/química , Propilaminas/química , Silanos/química , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura , Termogravimetria , Difração de Raios XRESUMO
N,N-dimethyltryptamine (DMT) is a potent hallucinogen found in beverages consumed in religion rituals and neo-shamanic practices over the world. Two of these religions, Santo Daime and União do Vegetal (UDV), are represented in countries including Australia, the United States and several European nations. In some of this countries there have been legal disputes concerning the legalization of ayahuasca consumption during religious rituals, a beverage rich in DMT. In Brazil, even children and pregnant women are legally authorized to consume ayahuasca in a religious context. A simple and low-cost method based on matrix solid-phase dispersion (MSPD) and gas chromatography with mass spectrometric detection (GC-MS) has been optimized for the determination of N,N-dimethyltryptamine in Mimosa tenuiflora inner bark. The experimental variables that affect the MSPD method, such as the amounts of solid-phase and herbal sample, solvent nature, eluate volume and NaOH concentration were optimized using an experimental design. The method showed good linearity (r = 0.9962) and repeatability (RSD < 7.4%) for DMT compound, with detection limit of 0.12 mg/g. The proposed method was used to analyze 24 samples obtained locally. The results showed that concentrations of the target compound in M. tenuiflora barks, ranged from 1.26 to 9.35 mg/g for these samples.
Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Mimosa/química , N,N-Dimetiltriptamina/análise , Extração em Fase Sólida/métodos , Limite de Detecção , Modelos Lineares , N,N-Dimetiltriptamina/isolamento & purificação , Casca de Planta/química , Reprodutibilidade dos TestesRESUMO
The consumption of ayahuasca, a hallucinogenic beverage used by indigenous communities in the Amazon, is increasing worldwide due to the expansion of syncretic religions founded in the north of Brazil in the first half of the twentieth century, such as Santo Daime and União do Vegetal. Another example is the jurema wine, a drink that originated from indigenous cultures of the northeast of Brazil. It is currently used for several religious practices throughout Brazil involving urban neo-shamanic rituals and syncretic Brazilian religions, such as Catimbó and Umbanda. Both plant products contain N,N-dimethyltryptamine which requires co-administration of naturally occurring monoamine oxidase inhibitors, for example ß-carboline derivatives, in order to induce its psychoactive effects in humans. This review explores the cultural use of tryptamines and ß-carbolines and focuses on the analytical techniques that have been recently applied to the determination of these compounds in ayahuasca, its analogues, and the plants used during the preparation of these beverages.