Novos adsorventes para aplicação na remoção de enxofre de combustíveis

Currently the market requires increasingly pure oil derivatives and, with that, comes the need for new methods for obtaining those products that are more efficient and economically viable. Considering the removal of sulfur from diesel, most refineries uses catalytic hydrogenation process, the hydrodesulfurization. These processes needs high energy content and high cost of production and has low efficiency in removing sulfur at low concentrations (below 500 ppm). The adsorption presents itself as an efficient and economically viable alternative in relation to the techniques currently used. With that, the main purpose of this work is to develop and optimize the obtaining of new adsorbents based on diatomite, modified with two non ionic surfactants microemulsions, adding efficiency to the material, to its application on removal of sulfur present in commercial diesel. Analyses were undertaken of scanning electron microscopy (SEM), x-ray diffraction (XRD), x-ray fluorescence (XRF), thermogravimetry (TG) and N2 adsorption (BET) for characterization of new materials obtained. The variables used for diatomite modification were: microemulsion points for each surfactant (RNX 95 and UNTL 90), microemulsion aqueous phase through the use or non-use of salts (CaCl2 and BaCl2), the contact time during the modification and the contact form. The study of adsorption capacity of materials obtained was performed using a statistical modeling to evaluate the influence of salt concentration in the aqueous phase (20 ppm to 1500 ppm), finite bath temperature (25 to 60° C) and the concentration of sulphur in diesel. It was observed that the temperature and the concentration of sulphur (300 to 1100 ppm) were the most significant parameters, in which increasing their values increase the ability of modified clay to adsorb the sulphur in diesel fuel. Adsorption capacity increased from 0.43 to mg/g 1.34 mg/g with microemulsion point optimization and with the addition of salts.

Características físico-químicas, sensoriais e perfil de ácidos graxos do leite de cabras saanen alimentadas com cactáceas

The objective of this research was to evaluate the influence of the supply of five types of native and exotic cacti Brazilian semiarid northeast on the sensory characteristics of milk of Saanen goats. Five multiparous goats were used with nine weeks of lactation, average live weight of 50 kg ± 4 kg., confined and distributed in a Latin square design 5 x 5 with five experimental diets and five periods. Each period lasted 17 days, with 10 days of adaptation to the diets of the animals and seven days for the data collection. The treatments were defined based on dry matter consisted of: 47.33 to 50.12% of a cactus (“Xiquexique”, “Mandacaru”, “Facheiro” or two species of forage cactus “Miúda” or “Orelha de Elefante Mexicana”) more 18.78 to 19.79% hay of plant “Sabiá” and 31.10 to 32.89% of concentrate. There was not effect of the experimental diets in the physical and chemical composition of milk for fat, total solids and salts, which showed mean values of 3.24%; 11.30% and 0.66%, respectively. However the protein, lactose, nonfat dry extract and freezing point were affected by diets. In the profile of fatty acids was higher concentration of fatty short and medium chain fatty acids, however, there were not changes between treatments, except for the butyric acid (C4:0), with mean values of 4.24% (“Orelha de Elefante Mexicana”) to 6.05% (“Facheiro”). The diets also did not provide sensory changes in milk for the parameters: odor, flavor, aftertaste and overall assessment. The use of the five cactus in the diet of dairy goats do not influence the sensory characteristics and lipid profile of milk. The physical and chemical composition of milk was showed within the minimum requirements of current legislation, except for nonfat dry extract and freezing point.

Tecnologia eletroquímica como tratamento alternativo de efluentes derivados da indústria têxtil e petroquímica

In this work, the treatment of wastewater from the textile industry, containing dyes as Yellow Novacron (YN), Red Remazol BR (RRB) and Blue Novacron CD (NB), and also, the treatment of wastewater from petrochemical industry (produced water) were investigated by anodic oxidation (OA) with platinum anodes supported on titanium (Ti/Pt) and boron-doped diamond (DDB). Definitely, one of the main parameters of this kind of treatment is the type of electrocatalytic material used, since the mechanisms and products of some anodic reactions depend on it. The OA of synthetic effluents containing with RRB, NB and YN were investigated in order to find the best conditions for the removal of color and organic content of the dye. According to the experimental results, the process of OA is suitable for decolorization of wastewaters containing these textile dyes due to electrocatalytic properties of DDB and Pt anodes. Removal of the organic load was more efficient at DDB, in all cases; where the dyes were degraded to aliphatic carboxylic acids at the end of the electrolysis. Energy requirements for the removal of color during OA of solutions of RRB, NB and YN depends mainly on the operating conditions, for example, RRB passes of 3.30 kWh m-3 at 20 mA cm-2 for 4.28 kWh m-3 at 60 mA cm-2 (pH = 1); 15.23 kWh m-3 at 20 mA cm-2 to 24.75 kWh m-3 at 60 mA cm-2 (pH 4.5); 10.80 kWh m-3 at 20 mA cm-2 to 31.5 kWh m-3 at 60 mA cm-2 (pH = 8) (estimated data for volume of treated effluent). On the other hand, in the study of OA of produced water effluent generated by petrochemical industry, galvanostatic electrolysis using DDB led to the complete removal of COD (98%), due to large amounts of hydroxyl radicals and peroxodisulphates generated from the oxidation of water and sulfates in solution, respectively. Thus, the rate of COD removal increases with increasing applied current density (15-60 mAcm-2 ). Moreover, at Pt electrode, approximately 50% removal of the organic load was achieved by applying from 15 to 30 mAcm-2 while 80% of COD removal was achieved for 60 mAcm-2 . Thus, the results obtained in the application of this technology were satisfactory depending on the electrocatalytic materials and operating conditions used for removal of organic load (petrochemical and textile effluents) as well as for the removal of color (in the case of textile effluents). Therefore, the applicability of electrochemical treatment can be considered as a new alternative like pretreatment or treatment of effluents derived from textiles and petrochemical industries.

Avaliação do ganho de peso de bebês prematuros em relação ao leite materno cru e leite pasteurizado

This study aims to evaluate the weight gain of premature newborns fed with breast milk from their mothers' from those that are fed with breast milk from the milk bank. The research is the quantitative, descriptive and observational kind. It was conducted in the Neonatal Intensive Care Unit and Housing from the Maternity Hospital Escola Januário Cicco (MEJC), that is a reference for high risk pregnancy and birth in Rio Grande do Norte. The premature newborns included were following these parameters: gestational age from 26 to 37 weeks, initially hospitalized at UTIN, with oral diet, by means by gavage, cup and/or suction. Studies with premature newborns with a zero diet longer than seven days or complications that interfered in the evaluation of weight gain were excluded from this study. The sample was selected for convenience and had data of all newborns hospitalized at UTIN from the May to June of 2014 time period, followed to their discharge, ended by August of 2014 and had the inclusion parameters of the study. From the period of the data collection, 60 premature newborns entered the maternity and 39 of those were the sample of research. The project was approved by the Research Ethics Committee from UFRN, under CAAE nº 0699.0.000.294-11. The data was analyzed by means of descriptive and deduced statistics. The results indicated that the involved in the study, were born from mother with average age of 25,36 years, with less than nine years education 21 (53,8%), had the family income less than a minimum wage 24 (61,5%). Among the newborn, the female gender predominated 20 (51,3%), had cesarean delivery 25 (64,1%), had moderate prematurity 29 (74,5%), more of 1.500g 22 (556,4%). The birth weight average was 1.608,49g. The total of diets were 9.994, and an average of 256 for each newborn, in a 32,12 days of hospitalization time period. Most of the diet supplies were from the breast milk bank (50,34%), however 56,4% of the newborns had most of the diet from their mothers' milked breast milk. It was detected that 38,5% of the newborns had, in some given moment, artificial milk. The daily weight gain average of all newborns was 2,59g, but 35% of them had an average above 10g per day. From the newborn's group (n=25) that had medium weight gain, only 9 of them (36,0%) received mainly their own mothers' milked breast milk. It's been conclusive that most of the premature newborns gained weight predominantly from diets from the breast milk of the Milk Bank, showing the need of a bigger incentive to exclusive breast feeding.

Avaliação da suplementação de vitamina E sobre a concentração de alfa-tocoferol no leite materno em mulheres com partos prematuros

The term vitamin E refers to a group of eight molecular compounds which differ in structure and bioavailability, and the RRR-alpha-tocopherol more biologically active form. The composition of vitamin E in breast milk undergoes variations during lactation, colostrum and milk richer in this micronutrient compared to transitional and mature milk. Newborns, especially premature infants are more susceptible to vitamin E deficiency and to prevent the damage caused by this deficiency has been proposed supplementation of neonates with this micronutrient, however, there is no consensus to carry out this intervention. Thus, maternal supplementation with RRRalpha-tocopherol in the postpartum period can be a good alternative to try to raise the alpha-tocopherol levels in breast milk and therefore provide the premature newborn adequate amounts of vitamin E. This study to evaluate the effect of supplementation with 400 UI acetate RRR-alpha-tocopherol in women with premature births, on the concentration of alpha-tocopherol in breast milk colostrum, transitional and mature. The study included 89 healthy adult women were enrolled in the control group (n = 51) and supplemented group (n = 38). Blood samples were collected and milk colostrum soon after birth (0h milk) twenty-four hours, new rate of colostrum milk was collected (24h milk). The transitional and mature milk were collected in seven days (7d milk) and thirty days (30d milk) after delivery, respectively. Supplementation in the supplemented group was held after the collection of blood and 0h milk. The alpha-tocopherol analyzes were performed by high-performance liquid chromatography. Serum levels of alpha-tocopherol less than 516 μg/dL were considered indicative of nutritional deficiency. The average concentration of alphatocopherol in the serum of the control group mothers was 1159.8 ± 292.4 μg/dL and the supplemented group was 1128.3 ± 407.2 μg/dL (p = 0.281). All women had nutritional status in vitamin E suitable. In both groups, it was observed that the concentration of vitamin E in colostrum milk was higher compared to transitional and mature milk. In the supplemented group, the concentration of alpha-tocopherol in the milk increased 60 % after supplementation, from 1339.3 ± 414.2 μg/dL (0h milk) to 2234.7 ± 997.3 μg/dL (24h milk). While the control group values in colostrum 0h and colostrum 24h were similar (p = 0.681). In the control group the follow-on milk alphatocopherol value was 875.3 ± 292.4 μg/dL and in the group supplemented 1352.8 ± 542.3 μg/dL, an increase of 35% in the supplemented group compared to control (p <0.001). In mature milk alpha-tocopherol concentrations between the control group (426.6 ± 187.5 μg/dL) and supplemented (416.4 ± 214.2 μg/dL) were similar (p = 0.853). Only 24h milk supplemented group answered the nutritional requirement of alpha-tocopherol (4 mg/day) of the newborn. These results show that the transport of this micronutrient for milk occurs in a controlled and limited way. Thus, the native vitamin E supplementation increases the concentration of alpha-tocopherol in colostrum and milk and transition does not influence the concentration in mature milk. Only the increase in colostrum milk was sufficient to meet the nutritional requirement of premature newborns.

Estudo de métodos de tratamento de efluentes (troca iônica e eletroquímico) separados e sequenciais para eliminação de derivados de petróleo

The produce of waste and the amount of the water produced coming from activities of petroleum production and extraction has been a biggest challenge for oil companies with respect to environmental compliance due to toxicity. The discard or the reuse this effluent containing organic compounds as BTEX (benzene, toluene, ethylbenzene and xylene) can cause serious environmental and human health problems. Thus, the objective this paper was study the performance of two process (separately and sequential) in one synthetic effluent for the benzene, toluene and xylene removal (volatile hydrocarbons presents in the produced water) through of electrochemical treatment using Ti/Pt electrode and exchange resin ionic used in the adsorption process. The synthetic solution of BTX was prepared with concentration of 22,8 mg L-1, 9,7 mg L-1 e 9,0 mg L-1, respectively, in Na2SO4 0,1 mol L-1. The experiments was developed in batch with 0.3 L of solution at 25ºC. The electrochemical oxidation process was accomplished with a Ti/Pt electrode with different current density (J = 10, 20 e 30 mA.cm-2). In the adsorption process, we used an ionic exchange resin (Purolite MB 478), using different amounts of mass (2,5, 5 and 10 g). To verify the process of technics in the sequential treatment, was fixed the current density at 10 mA cm-2 and the resin weight was 2.5 g. Analysis of UV-VIS spectrophotometry, chemical oxygen demand (COD) and gas chromatography with selective photoionization detector (PID) and flame ionization (FID), confirmed the high efficiency in the removal of organic compounds after treatment. It was found that the electrochemical process (separate and sequential) is more efficient than absorption, reaching values of COD removal exceeding 70%, confirmed by the study of the cyclic voltammetry and polarization curves. While the adsorption (separately), the COD removal did not exceed 25,8%, due to interactions resin. However, the sequential process (electrochemical oxidation and adsorption) proved to be a suitable alternative, efficient and cost-effectiveness for the treatment of effluents petrochemical.

Distribuição de derivados de petróleo por redes de polidutos: uma abordagem através de algoritmos evolucionários híbridos para um problema triobjetivo

An important problem faced by the oil industry is to distribute multiple oil products through pipelines. Distribution is done in a network composed of refineries (source nodes), storage parks (intermediate nodes), and terminals (demand nodes) interconnected by a set of pipelines transporting oil and derivatives between adjacent areas. Constraints related to storage limits, delivery time, sources availability, sending and receiving limits, among others, must be satisfied. Some researchers deal with this problem under a discrete viewpoint in which the flow in the network is seen as batches sending. Usually, there is no separation device between batches of different products and the losses due to interfaces may be significant. Minimizing delivery time is a typical objective adopted by engineers when scheduling products sending in pipeline networks. However, costs incurred due to losses in interfaces cannot be disregarded. The cost also depends on pumping expenses, which are mostly due to the electricity cost. Since industrial electricity tariff varies over the day, pumping at different time periods have different cost. This work presents an experimental investigation of computational methods designed to deal with the problem of distributing oil derivatives in networks considering three minimization objectives simultaneously: delivery time, losses due to interfaces and electricity cost. The problem is NP-hard and is addressed with hybrid evolutionary algorithms. Hybridizations are mainly focused on Transgenetic Algorithms and classical multi-objective evolutionary algorithm architectures such as MOEA/D, NSGA2 and SPEA2. Three architectures named MOTA/D, NSTA and SPETA are applied to the problem. An experimental study compares the algorithms on thirty test cases. To analyse the results obtained with the algorithms Pareto-compliant quality indicators are used and the significance of the results evaluated with non-parametric statistical tests.

Síntese e reatividade de derivados de quinoxalina visando aplicações como quimiossensores e estudo cinético por análise de imagens

Synthesis of heterocyclic compounds, as quinoxaline derivatives, has being shown to be relevant and promissor due to expressive applications in biological and technological areas. This work was dedicated to the synthesis, characterization and reactivity of quinoxaline derivatives in order to obtain new chemosensors. (L)-Ascorbic acid (1) and 2,3-dichloro-6,7- dinitroquinoxalina (2) were explored as synthetic precursors. Starting from synthesis of 1 and characterization of compounds derived from (L)-ascorbic acid, studies were performed investigating the application of products as chemosensors, in which compound 36 demonstrated selective affinity for Cu2+ íons in methanolic solution, by naked-eye (colorimetric) and UVvisible analyses. Further, initial analysis suggests that 39 a Schiff’s base derived from 36 also presents this feature. Five quinoxaline derivatives were synthesized from building block 2 through nucleophilic aromatic substitution by aliphatic amines, in which controlling the experimental conditions allows to obtain both mono- and di-substituted derivatives. Reactivity studies were carried out with two purposes: i) investigate the possibility of 47 compound being a chemosensor for anion, based on its interaction with sodium hydroxide in DMSO, using image analysis and UV-visible spectroscopy; ii) characterize kinetically the conversion of compound 44 into 46 based on RGB and multivariate image analysis from TLC data, as a simple and inexpensive qualitative and quantitative tool.

Dextranas e seus derivados fosforilados: obtenção e avaliação do potencial antioxidante, imunomodulatório e anticoagulante

Glucans are polysaccharides with different pharmacological and biological activities described. However, there are some reports about the activities of the glucan type α (alpha). In this context, a group of α-D-glucans called dextrans extracted from Leuconostoc mesenteroides bacteria, with molecular weights of 10 (D10), 40 (D40) and 147 (D147) kDa and their phosphorylated derivatives P10, P40 and P147, were evaluated as for their antioxidant, anticoagulant and immunomodulatory potential for the first time, in order to elucidate compounds with potent activities and low toxicity. Infrared spectroscopy analysis, monosaccharide composition and chemical dosages showed that these dextrans are the same polysaccharide, but with different molecular weights, besides confirming the success of phosphorylation. None presented with anticoagulant features. The reducing power test showed that D147 was twice as potent as other dextrans. On the other hand, all six samples showed similar activity (50%) when it came to scavenging the OH radical. To the superoxide ion scavenging, only D10 had a pronounced activity (50%). D40 was the single native dextran that presented with immunomodulatory features since it double stimulated the proliferation of murine macrophages (RAW 264.7) and double the release of nitric oxide by the cells, both in the absence and presence of lipopolysaccharides (LPS). In addition, D40 showed a greater scavenging activity (50%) for the hydrogen peroxide, which caused it to also be the more potent dextran when it came to inhibiting lipid peroxidation (70%). On other hand, P147 showed the highest iron and copper ion chelation activity (~85%). P10 proved be the most effective compound to macrophage proliferation. The results point toward dextrans with a 40 kDa weight as being ideal for antioxidant and immunomodulatory use, could be supplemented with phosphorylated derivatives. However, future studies with the D40 and other similarly dextrans are to confirm this hypothesis.

Ocorrência de leite instável na região semiárida do Rio Grande do Norte e sua correlação com a qualidade do leite

The unstable non acid milk (UNAM) is characterized by coagulation in the alcohol test and wanted acidity (14-18°D). Among Brazilian regions, the South and Southeast have the highest occurrence of LINA, which has been causing problems for both producers and for industries, due to the disposal or undervaluation of milk. In the Northeast there are few studies that indicate their occurrence and quality. The objective of this study was to identify the occurrence of unstable non-acid milk in the west and central mesoregions of Rio Grande do Norte, determine their physicochemical characteristics, test alcoholic graduations and evaluate their correlation with the quality of milk. 176 raw milk samples were analyzed in the period from September to December /2014 from 23 APASA’s cooling tanks, located in 7 cities of west and central mesoregions RN. The samples were collected in duplicate, one sample used for alcohol testing at 68, 72 and 76%, measurement of pH, acidity, electrical conductivity and boiling proof, made in LABOLEITE / UFRN; and the other sample containing Bronopol® preservative, was sent to the APCBRH (Cattle Breeders Association Paranaense Holstein) laboratory in Curitiba-PR, which were analyzed fat, protein, total solids, lactose, casein, urea nitrogen and somatic cell count. The test alcohol samples disapproved 31.82%, of which 30% proved to be non-acid, and 30% had high acidity. The samples were divided into three classes: Stable Milk, UNAM and acid milk. 3% Tukey test was used for comparison of stable milk components and UNAM and there was no significant difference between them. Both classes obtained averages within the standard required by IN 62. The average value of electric conductivity was 4.84 mS/cm for stable milk, 4.55 mS/cm for unstable and acid milk and 4.53 mS/cm for non-acid unstable milk. The electrical conductivity was positively correlated with alcohol stability of milk and negative correlation with acidity and pH. Could not observe direct relationship between the electrical conductivity and the somatic cell count.The boiling test was negative for all samples UNAM. It can be concluded that the incidence of UNAM in the studied region is low, although the predisposing factors such as heat stress, drought and nutritional deficiency. In conclusion, the UNAM has quality similar to stable milk, conform the norms required by Agriculture Ministry, and with adequate thermal stability, which proves that there is no reason to reject this milk by industry.

Novos protocolos teóricos utilizados nos estudos das ligações hidrogênio-hidrogênio, na estabilidade do tetraedrano, seus derivados e das reações de diels-alder e na quantificação da afinidade de fármacos

This thesis was performed in four chapters, at the theoretical level, focused mainly on electronic density. In the first chapter, we have applied an undergraduate minicourse of Diels-Alder reaction in Federal University of Rio Grande do Norte. By using computational chemistry tools students could build the knowledge by themselves and they could associate important aspects of physical-chemistry with Organic Chemistry. In the second chapter, we studied a new type of chemical bond between a pair of identical or similar hydrogen atoms that are close to electrical neutrality, known as hydrogen-hydrogen (H-H) bond. In this study performed with complexed alkanes, provides new and important information about their stability involving this type of interaction. We show that the H-H bond playing a secondary role in the stability of branched alkanes in comparison with linear or less branched isomers. In the third chapter, we study the electronic structure and the stability of tetrahedrane, substituted tetrahedranes and silicon and germanium parents, it was evaluated the substituent effect on the carbon cage in the tetrahedrane derivatives and the results indicate that stronger electron withdrawing groups (EWG) makes the tetrahedrane cage slightly unstable while slight EWG causes a greater instability in the tetrahedrane cage. We showed that the sigma aromaticity EWG and electron donating groups (EDG) results in decrease and increase, respectively, of NICS and D3BIA aromaticity indices. In addition, another factor can be utilized to explain the stability of tetra-tert-butyltetrahedrane as well as HH bond. GVB and ADMP were also used to explain the stability effect of the substituents bonded to the carbon of the tetrahedrane cage. In the fourth chapter, we performed a theoretical investigation of the inhibitory effect of the drug abiraterone (ABE), used in the prostate cancer treatment as CYP17 inhibitor, comparing the interaction energies and electron density of the ABE with the natural substrate, pregnenolone (PREG). Molecular dynamics and docking were used to obtain the CYP1ABE and CYP17-PREG complexes. From molecular dynamics was obtained that the ABE has higher diffusion trend water CYP17 binding site compared to the PREG. With the ONIOM (B3LYP:AMBER) method, we find that the interaction electronic energy of ABE is 21.38 kcal mol-1 more stable than PREG. The results obtained by QTAIM indicate that such stability is due a higher electronic density of interactions between ABE and CYP17

Qualidade do leite de búfala (Bubalus bubalis) suplementada com selênio

This study aimed to evaluate the effect of diet with selenium on the physico-chemical composition and somatic cell count of buffalo milk, and check the selenium waste in milk and minas kind fresh cheese. For the analysis of physical-chemical composition and SCC were used 2264 buffalo milk data from the Murrah, belonging to Tapuio Ltda, located in the agreste region of the state of Rio Grande do Norte, in the period 2010 to 2014. To check the amount of selenium residue in buffalo milk and fresh cheese mines were used 100 Murrah buffaloes divided into 5 lots. The batches were formed according to the production levels of animals, wherein the amount of concentrate fed varied within each lot, which received 0.08 ppm / Se / kg of concentrate. Was collected from 300 ml of tank milk from and each lot, as well as 300 gr minas cheese, from August to November 2014, with the collection of lots held only in the month of November. The samples were sent to the Pernambuco Tecnology Institute for selenium residue analysis. The effect of the seasons was contrasted in two ways, namely: Spring, Summer, Autumn and Winter season or drought and rainy season. The analyzes statistics were performed using the procedures available in the software SAS® (SAS, 2002). Selenium level provided to the animals in this study was not significant to the point of detection of their residue in milk and the cheeses. However, it influences the reduction of the CCS. The milk characteristics were not affected by selenium use only the seasons.

Qualidade do leite de búfala (Bubalus bubalis) suplementada com selênio

This study aimed to evaluate the effect of diet with selenium on the physico-chemical composition and somatic cell count of buffalo milk, and check the selenium waste in milk and minas kind fresh cheese. For the analysis of physical-chemical composition and SCC were used 2264 buffalo milk data from the Murrah, belonging to Tapuio Ltda, located in the agreste region of the state of Rio Grande do Norte, in the period 2010 to 2014. To check the amount of selenium residue in buffalo milk and fresh cheese mines were used 100 Murrah buffaloes divided into 5 lots. The batches were formed according to the production levels of animals, wherein the amount of concentrate fed varied within each lot, which received 0.08 ppm / Se / kg of concentrate. Was collected from 300 ml of tank milk from and each lot, as well as 300 gr minas cheese, from August to November 2014, with the collection of lots held only in the month of November. The samples were sent to the Pernambuco Tecnology Institute for selenium residue analysis. The effect of the seasons was contrasted in two ways, namely: Spring, Summer, Autumn and Winter season or drought and rainy season. The analyzes statistics were performed using the procedures available in the software SAS® (SAS, 2002). Selenium level provided to the animals in this study was not significant to the point of detection of their residue in milk and the cheeses. However, it influences the reduction of the CCS. The milk characteristics were not affected by selenium use only the seasons.

Desenvolvimento de métodos para quantificação de benzilpenicilina em medicamentos veterinários e seus resíduos em leite bovino e caprino por UFLC-DAD

The Benzylpenicillin (PENG) have been as the active ingredient in veterinary medicinal products, to increase productivity, due to its therapeutic properties. However, one of unfortunate quality and used indiscriminately, resulting in residues in foods exposed to human consumption, especially in milk that is essential to the diet of children and the ageing. Thus, it is indispensable to develop new methods able to detect this waste food, at levels that are toxic to human health, in order to contribute to the food security of consumers and collaborate with regulatory agencies in an efficient inspection. In this work, were developed methods for the quality control of veterinary drugs based on Benzylpenicillin (PENG) that are used in livestock production. Additionally, were validated methodologies for identifying and quantifying the antibiotic residues in milk bovine and caprine. For this, the analytical control was performed two steps. At first, the groups of samples of medicinal products I, II, III, IV and V, individually, were characterized by medium infrared spectroscopy (4000 – 600 cm-1). Besides, 37 samples, distributed in these groups, were analyzed by spectroscopy in the ultraviolet and near infrared region (UV VIS NIR) and Ultra Fast Liquid Chromatograph coupled to linear arrangement photodiodes (UFLC-DAD). The results of the characterization indicated similarities, between PENG and reference standard samples, primarily in regions of 1818 to 1724 cm-1 of ν C=O that shows primary amides features of PENG. The method by UFLC-DAD presented R on 0.9991. LOD of 7.384 × 10-4 μg mL-1. LOQ of 2.049 × 10-3 μg mL-1. The analysis shows that 62.16% the samples presented purity ≥ 81.21%. The method by spectroscopy in the UV VIS NIR presented medium error ≤ 8 – 12% between the reference and experimental criteria, indicating is a secure choice for rapid determination of PENG. In the second stage, was acquiring a method for the extraction and isolation of PENG by the addition of buffer McIlvaine, used for precipitation of proteins total, at pH 4.0. The results showed excellent recovery values PENG, being close to 92.05% of samples of bovine milk (method 1). While samples of milk goats (method 2) the recovery of PENG were 95.83%. The methods for UFLC-DAD have been validated in accordance with the maximum residue limit (LMR) of 4 μg Kg-1 standardized by CAC/GL16. Validation of the method 1 indicated R by 0.9975. LOD of 7.246 × 10-4 μg mL-1. LOQ de 2.196 × 10-3 μg mL-1. The application of the method 1 showed that 12% the samples presented concentration of residues of PENG > LMR. The method 2 indicated R by 0.9995. LOD 8.251 × 10-4 μg mL-1. LOQ de 2.5270 × 10-3 μg mL-1. The application of the method showed that 15% of the samples were above the tolerable. The comparative analysis between the methods pointed better validation for LCP samples, because the reduction of the matrix effect, on this account the tcalculs < ttable, caused by the increase of recovery of the PENG. In this mode, all the operations developed to deliver simplicity, speed, selectivity, reduced analysis time and reagent use and toxic solvents, particularly if compared to the established methodologies.

Desenvolvimento de métodos para quantificação de benzilpenicilina em medicamentos veterinários e seus resíduos em leite bovino e caprino por UFLC-DAD

The Benzylpenicillin (PENG) have been as the active ingredient in veterinary medicinal products, to increase productivity, due to its therapeutic properties. However, one of unfortunate quality and used indiscriminately, resulting in residues in foods exposed to human consumption, especially in milk that is essential to the diet of children and the ageing. Thus, it is indispensable to develop new methods able to detect this waste food, at levels that are toxic to human health, in order to contribute to the food security of consumers and collaborate with regulatory agencies in an efficient inspection. In this work, were developed methods for the quality control of veterinary drugs based on Benzylpenicillin (PENG) that are used in livestock production. Additionally, were validated methodologies for identifying and quantifying the antibiotic residues in milk bovine and caprine. For this, the analytical control was performed two steps. At first, the groups of samples of medicinal products I, II, III, IV and V, individually, were characterized by medium infrared spectroscopy (4000 – 600 cm-1). Besides, 37 samples, distributed in these groups, were analyzed by spectroscopy in the ultraviolet and near infrared region (UV VIS NIR) and Ultra Fast Liquid Chromatograph coupled to linear arrangement photodiodes (UFLC-DAD). The results of the characterization indicated similarities, between PENG and reference standard samples, primarily in regions of 1818 to 1724 cm-1 of ν C=O that shows primary amides features of PENG. The method by UFLC-DAD presented R on 0.9991. LOD of 7.384 × 10-4 μg mL-1. LOQ of 2.049 × 10-3 μg mL-1. The analysis shows that 62.16% the samples presented purity ≥ 81.21%. The method by spectroscopy in the UV VIS NIR presented medium error ≤ 8 – 12% between the reference and experimental criteria, indicating is a secure choice for rapid determination of PENG. In the second stage, was acquiring a method for the extraction and isolation of PENG by the addition of buffer McIlvaine, used for precipitation of proteins total, at pH 4.0. The results showed excellent recovery values PENG, being close to 92.05% of samples of bovine milk (method 1). While samples of milk goats (method 2) the recovery of PENG were 95.83%. The methods for UFLC-DAD have been validated in accordance with the maximum residue limit (LMR) of 4 μg Kg-1 standardized by CAC/GL16. Validation of the method 1 indicated R by 0.9975. LOD of 7.246 × 10-4 μg mL-1. LOQ de 2.196 × 10-3 μg mL-1. The application of the method 1 showed that 12% the samples presented concentration of residues of PENG > LMR. The method 2 indicated R by 0.9995. LOD 8.251 × 10-4 μg mL-1. LOQ de 2.5270 × 10-3 μg mL-1. The application of the method showed that 15% of the samples were above the tolerable. The comparative analysis between the methods pointed better validation for LCP samples, because the reduction of the matrix effect, on this account the tcalculs < ttable, caused by the increase of recovery of the PENG. In this mode, all the operations developed to deliver simplicity, speed, selectivity, reduced analysis time and reagent use and toxic solvents, particularly if compared to the established methodologies.