Aplicação de métodos quimiométricos na otimização da extração de Ca, Mg, K, Fe, Zn, Cu e Mn em folhas de braquiária

This work applied a 2² factorial design to the optimization of the extraction of seven elements (calcium, magnesium, potassium, iron, zinc, copper and manganese) in brachiaria leaves, determined by flame atomic absorption spectrometry. The factors sample mass and digestion type were evaluated at two levels: 200/500 mg, and dry/wet, respectively. Principal component analysis allowed simultaneous discrimination of all the significant effects in one biplot. Wet digestion and mass of 200 mg were considered the best conditions. The decrease of 60% in sample mass allowed to save costs and reagents. The method was validated through the estimation of figures of merit.

Modelagem termodinâmica por extração por solvente de metais divalentes em meio sulfato usando D2EHPA

The extraction of divalent metals (Mn2+, Ni2+, Co2+ and Cu2+) in the system MSO4 - H2SO4 - H2O - D2EHPA in isoparaffin (17/21) was studied by a thermodynamic model based on chemical equilibria with mass and charge balance equations. The activity coefficients of all solutes in the aqueous phase were calculated by Davies equation. By applying this model, the equilibrium concentrations of solutes were calculated from de concentration of divalent metals and pH. The predicted distribution coefficients for the divalents metals were in good agreement with experimental results.

Extração sequencial de zinco e cobre em solos tratados com lodo de esgoto e composto de lixo

This work aimed to access the contents and chemical forms and to estimate mobility and availability of cooper and zinc in samples from two soils (Haplortox and Paleudult) previously treated with doses of sewage sludge (SS) and municipal solid waste compost (MSWC), besides a control treatment. Largest percentages of Cu and Zn were determined in the organic matter fraction. Zn showed higher percentages of soluble and exchangeable fractions than Cu. Treatments with SS showed higher potential of Cu and Zn availability. Modifications in soil attributes due to residue application affected metal mobility and availability indexes.

Composição química e avaliação da atividade antimicrobiana do óleo essencial das folhas de Piper malacophyllum (C. Presl.) C. DC.

This work reports the chemical composition as well as the antibacterial, antifungal and antiparasitic activities of the leaf essential oil from Piper malacophyllum. The oil was extracted by hydrodistillation and analyzed by GC-FID, GC-MS and polarimetry. Among the 28 compounds identified, (+)-camphor was the major constituent. The essential oil showed activity against most of the microorganisms tested, especially antifungal action, with a MIC of 500 µg mL-1 against Trichophyton mentagrophytes and Cryptococcus neoformans. This is the first study reporting the composition and biological properties of leaf essential oil from P. malacophyllum.

Determinação de bifenilos policlorados em milho através de extração em fase sólida seguida de cromatografia a gás acoplada à espectrometria de massas

This paper describes an analytical method for analyzing polychlorinated biphenyls in corn samples using solid phase extraction (SPE) followed by determination by GC-MS. All calibration curves proved linear (r> 0.99). Recoveries ranged between 74.1 and 110.6% with relative standard deviation lower than 20% for all compounds. The limits of quantitation for the method were between 0.025 and 0.1 ng g-1. Of the 51 samples analyzed, PCB 180 showed the highest frequency, being detected in more than 39%, followed by PCB 138, detected in more than 33% of samples.

Biomassa em aula prática de Química Orgânica Verde: cravo-da-índia como fonte simultânea de óleo essencial e de furfural

This work presents an optimized integrated experiment for isolation of clove bud essential oil, rich in eugenol, and subsequent utilization of the solid residue for furfural synthesis. The operationally simple laboratory protocols and utilization of water as a solvent in both operations, plus the use of biomass as the starting material for preparation of versatile intermediates in organic synthesis, make the experiments attractive for undergraduate experimental organic chemistry courses in the context of green chemistry. In addition, this is the first description of the use of biomass (clove bud) in the simultaneous preparation of two chemical feedstocks, eugenol and furfural, on experimental organic chemistry courses.

Craqueamento termo-catalítico da mistura óleo de fritura usado-lodo de estamparia têxtil para a produção de óleo com baixo índice de acidez

In this work, cracking experiments were performed to carry out the thermal conversion of the mixture of used frying oil and textile stamping sludge in continuous reactor. The textile stamping sludge was used to catalyze the reaction of thermal cracking. The physical and chemical properties of the oil produced were analyzed. Among the results of this analysis the level of acidity in the range of 12 mg KOH/g stands out. Low levels of acidity as this particular mean better quality oil. In this regard it is important that further researches on processes of conversion of residual oil occur.

Caracterização composicional e transesterificação de óleo de microalga: uma abordagem computacional

A procedure for compositional characterization of a microalgae oil is presented and applied to investigate a microalgae based biodiesel production process through process simulation. The methodology consists of: proposing a set of triacylglycerides (TAG) present in the oil; assuming an initial TAG composition and simulating the transesterification reaction (UNISIM Design, Honeywell) to obtain FAME characterization values (methyl ester composition); evaluating deviations of experimental from calculated values; minimizing the sum of squared deviations by a non-linear optimization algorithm, with TAG molar fractions as decision variables. Biodiesel from the characterized oil is compared to a rapeseed based biodiesel.

Epoxidação do óleo de soja com o sistema catalítico [MoO2(acac)2]/TBHP EM [bmim][PF6]

Epoxidation of soybean oil was investigated using 1-n-butyl-3-methylimidazolium hexafluorophosphate [bmim][PF6] ionic liquid as biphasic medium with molybdenum(VI) acetylacetonate complex and tert-butyl hydroperoxide TBHP as oxidizing agent. Reaction conditions were molar ratio TBHP:number of double bonds of oil:catalyst of 100:100:1, reaction temperature of 60 ºC and reaction time between 2 and 24 h. The proposed system showed catalytic activity for epoxidation reactions under tested conditions. Reuse of ionic liquid/catalyst system for epoxidation reactions was also investigated. Evaluation of epoxidation observed in this catalytic system was done by quantitative ¹H NMR data.

Extração de ácido trans-trans mucônico urinário com polímeros de impressão molecular e análise por cromatografia gasosa: espectrometria de massas

This paper describes selective molecularly imprinted solid-phase extraction of ttMA from urine samples followed by derivatization and analysis by gas chromatography/mass spectrometry (GC/MS). The analytical calibration curve ranged from 0.3 to 7.0 mg L-1 (r = 0.999) and the limit of quantitation (LOQ) was 0.3 mg L-1. The method was applied for the determination of ttMA in urine samples from smokers and concentrations detected ranged from < LOQ to 1.64 mg L-1. Thus, the proposed method proved adequate for the determination of urinary ttMA in the biomonitoring of occupational exposure to low levels of benzene.

Extração/pré-concentração de íons cobre no ponto nuvem explorando a formação de complexos com DMIT [4,5-dimercapto-1,3-ditiol-2-tionato]

The present study proposes a method for cloud point preconcentration of copper ions at pH 2.0 based on complexes formed with [4,5-dimercapto-1,3-dithyol-2-thionate] and subsequent determination by flame atomic absorption spectrometry (FAAS). Under optimal analytical conditions, the method provided limits of detection of 0.84 and 0.45 µg L-1, by preconcentrating 12.0 and 24.0 mL of sample, respectively. The method was applied for copper determination in water samples, synthetic saliva, guarana powder, tea samples and soft drinks and the accuracy was assessed by analyzing the certified reference materials Dogfish Liver (DOLT-4) and Lobster Hepatopancreas (TORT-2).

Avaliação de métodos de extração para a determinação de cromo e níquel em formulações farmacêuticas e em matérias-primas usadas na fabricação de medicamentos à base de cefalexina e ciprofloxacino

This paper reports the evaluation of extraction strategies for the treatment of medicine samples to determine chromium and nickel by GFAAS. Different approaches for extraction were evaluated and the most efficient involved magnetic stirring. The metals were quantitatively extracted by stirring 0.20 g samples with 25 mL of 2.0 mol L-1 HCl solution for 60 min. The developed method was successfully applied for the determination of Cr and Ni in tablets containing antibiotics and raw materials, with cephalexin and ciprofloxacin as active ingredients.

Determinação de Cu, Fe, Mn, Zn e do teor de proteína total em amostras de trigo e soja após procedimento de extração sequencial

A sequential extraction procedure was applied to wheat and soybean seed samples. The total protein content (determined by two distinct methods: Bradford and bicinchoninic acid-BCA) and distribution of Cu, Fe, Mn and Zn in each fraction was determined. The sequential extraction employed four different solutions: water, 0.5 mol L-1 NaCl, ethanol/water (70:30 v v-1) and 0.5 mol L-1 NaOH. For both samples, the highest concentration of metals was observed in those extracts associated with globulin-type proteins using NaCl solution. Regarding protein content, higher levels were obtained using the BCA method.

Análise de agrotóxicos em água usando extração líquido-líquido com partição em baixa temperatura por cromatografia líquida de alta eficiência

This study optimized and validated the liquid-liquid extraction technique with partition at low temperature (LLE-PLT) for identification and quantification of four pesticides (chlorpyrifos, λ-cyhalothrin, permethrin, bifenthrin) in water samples. Analyses were performed by HPLC-UV. The technique was efficient for pesticide recovery with extraction exceeding 86%. Chromatographic response was linear for the four compounds in the 10-45 µg L-1 range, with correlation coefficients greater than 0.99. Limits of detection and quantitation were less than 3.5 µg L-1 and equal to 10 µg L-1, respectively. The proposed method was applied to 29 water samples from the Jaíba Project in northern Minas Gerais.

Constituintes químicos de Capraria biflora (Scrophulariaceae) e atividade larvicida de seu óleo essencial

Analysis of essential oil from fresh leaves of Capraria biflora allowed identification of fourteen essential oil constituents among which thirteen are sesquiterpene compounds, and α-humulene (43.0%) the major constituent. The essential oil was tested for larvicidal activity against Aedes aegypti showing good activity, with LC50 73.39 µg/mL (2.27 g/mL). Chromatographic studies of extracts from roots and stems allowed the isolation of five compounds: naphthoquinone biflorin, sesquiterpene caprariolide B, the steroid β-sitosterol, the carbohydrate D-mannitol and iridoid myopochlorin first reported in the species C. biflora. The structures of compounds were characterized by spectroscopic data, IR, MS, NMR13C, NMR¹H, NOE, HSQC and HMBC.