Experimental Analyses and Predictive Modelling of Ultrasonic Welding Parameters for Enhancing Smart Textile Fabrication.

This study aims to illustrate the design, fabrication, and optimisation of an ultrasonic welding (UW) machine to join copper wires with non-woven PVC textiles as smart textiles. The study explicitly evaluates UW parameters' impact on heat generation, joint strength, and electrical properties, with a comprehensive understanding of the process dynamics and developing a predictive model applicable to smart textiles. The methodological approach involved designing and manufacturing an ultrasonic piezoelectric transducer using ABAQUS finite element analyses (FEA) software and constructing a UW machine for the current purpose. The full factorial design (FFD) approach was employed in experiments to systematically assess the influence of welding time, welding pressure, and copper wire diameter on the produced joints. Experimental data were meticulously collected, and a backpropagation neural network (BPNN) model was constructed based on the analysis of these results. The results of the experimental investigation provided valuable insights into the UW process, elucidating the intricate relationship between welding parameters and heat generation, joint strength, and post-welding electrical properties of the copper wires. This dataset served as the basis for developing a neural network model, showcasing a high level of accuracy in predicting welding outcomes compared to the FFD model. The neural network model provides a valuable tool for controlling and optimising the UW process in the realm of smart textile production.

Multivariate optimization of dispersive liquid-liquid microextraction using ionic liquid for the analysis of ultraviolet filters in natural waters.

In this work, a vortex-assisted dispersive liquid-liquid microextraction method, using an ionic liquid as the extracting solvent was developed, for the simultaneous analysis of three UV filters in different water samples. The extracting and dispersive solvents were selected in a univariate way. Then, the parameters such as the volume of the extracting and dispersive solvents, pH and ionic strength were evaluated using a full experimental design 24, followed by Doehlert matrix. The optimized method consisted of 50 µL of extracting solvent (1-octyl-3-methylimidazolium hexafluorophosphate), 700 µL of dispersive solvent (acetonitrile) and pH of 4.5. When combined with high-performance liquid chromatography, the method limit of detection ranged from 0.3 to 0.6 µg L-1, enrichment factors between 81 and 101%, and the relative standard deviation between 5.8 and 10.0%. The developed method demonstrated effectiveness in concentrating UV filters in both river and seawater samples, being a simple and efficient option for this type of analysis.

Bio-Based Composites for Light Automotive Parts: Statistical Analysis of Mechanical Properties; Effect of Matrix and Alkali Treatment in Sisal Fibers.

Composites based on virgin and recycled polypropylene (PP and rPP) reinforced with 15 wt% sisal fibers, with and without alkali treatment, were prepared by compression molding in a mat composed of a three-layer sandwich structure. The sisal was characterized by Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The composites were characterized according to physical and mechanical properties. Additionally, a factorial experimental design was used to statistically evaluate the mechanical properties of the composite. The FTIR and XRD indicated the partial removal of amorphous materials from the surface of the sisal after alkali treatment. The composites' density results varied from 0.892 to 0.927 g·cm-3, which was in the desirable range for producing lightweight automotive components. A slight decrease in the hardness of the pure rPP and rPP composites in relation to the PP was observed. The water absorption was higher in rPP composites, regardless of the chemical treatment. Moreover, the impact resistance of PP and its composites was higher than the values for rPP. Statistical analysis showed that the alkali treatment was a significant factor for the hardness of the rPP and PP composites, and that the addition of the sisal layer was relevant to improve the impact resistance of the composites.

Response Surface Methodology for Optimization of Buspirone Hydrochloride-Loaded In Situ Gel for Pediatric Anxiety.

The purpose of the current investigation was to formulate, assess, and optimize oral in situ gels of buspirone hydrochloride (BH) with the specific end goal of expanding the time the medication spends in the stomach, thereby ensuring an extended medication discharge. This would allow the use of a once-a-day dose of liquid BH formulations, which is ideal for the treatment of pediatric anxiety. In situ gels loaded with BH were prepared using various concentrations of sodium alginate (Na alg.), calcium chloride (CaCl2), and hydroxypropyl methylcellulose (HPMC K15M). The in situ gels exhibited the desired consistency, drug distribution, pH, ability to form gel, and prolonged drug release in vitro. The (33) full factorial design was utilized for the revealing of the ideal figures for the selected independent variables, Na alg. (X1), HPMC (X2), and CaCl2 (X3) based on measurements of the viscosity (Y1) and percentage drug release after 6 h (Y2). A pharmacokinetic study of the optimum formulation on rabbits was also performed. The formulation containing 2% of Na alg., 0.9% of HPMC-K15M, and 0.1125% of CaCl2 was selected as the ideal formulation, which gave the theoretical values of 269.2 cP and 44.9% for viscosity and percentage of drug released after 6 h, respectively. The pharmacokinetic study showed that the selected oral Na alg. in situ gel formulation displayed a prolonged release effect compared to BH solution and the marketed tablet (Buspar®), which was confirmed by the low Cmax and high Tmax values. The optimum oral Na alg. in situ gel showed a 1.5-fold increment in bioavailability compared with the drug solution.

Toxicity treatment of tobacco wastes using experimental design by filamentous fungi.

Cigarette product waste contains toxic chemicals, including human carcinogens, which leach into and accumulate in the environment and represent a current environmental problem neglected for too long. This study aimed to select filamentous fungi capable of decreasing tobacco extract toxicity as an alternative to a future bioremediation process. The 38 isolates obtained from Culture collection of microorganisms to biotechnological and environmental importance - CCMIBA (Brazil) were cultivated in yeast extract (10 g.L-1) and dextrose (10 g.L-1) containing cigarette tobacco extract (200 mL.L-1) for seven days at 28 °C on a rotary shaker at 150 rpm. The fungal growth rate was determined to infer fungal tolerance to tobacco extract, and supernatants from cultivated fungi were used to run the toxicity test using Allium cepa assay. The Fusarium sp. strain I.17, isolated from cigarette waste, was the only lineage capable of growing in 20% (v/v) of cigarette tobacco extract, allowed the onions to root, and was selected for optimization. Initially, for the experimental design to selected fungus, a fractional factorial experimental design 25-1 was used to examine the effects of yeast extract, cigarette tobacco extract concentration, dextrose, copper sulfate and pH fungal cultivation. The supernatants of these assays were used to run the toxicity test, and yeast extract and copper sulfate were statistically significant in the fungal growth for the decreasing toxicity process and this variable as were select to central composite design. The highest concentration of yeast extract negatively influenced the toxicity decrease, 0.5% of yeast extract in the culture media is the maximum concentration to achieve the best result and to copper sulfate the best result was using 10 µmol.L-1. In conclusion, the experimental design optimized more than seven times the efficiency of tobacco toxicity reducing, resulting in more than 50% of onion root growth, demonstrating the methodology success. And ITS region was used to taxonomy and molecular phylogeny of the isolate Fusarium sp. strain I.17. These results suggest that Fusarium sp. strain I.17 can be used as a potential microorganism to toxicity treatment of cigarette wastes, minimizing the environmental impact of direct burning.

Development and characterization of biopolymer films based on bocaiuva (Acromonia aculeata) flour.

This work aimed to produce films based on bocaiuva flour (Acrocomia aculeata) by the casting method, and to characterise them. All obtained films were visually symmetrical, without ruptures or blistering and visually homogeneous, easy to handle with a yellowish colouration. The addition of glycerol allowed greater flexibility to the films. The tensile strength and the elongation increase as the concentration of flour increased (2.04 g 100 mL-1). The addition of oily phases increases the elongation, indicating that the essential oil incorporated into the films acted as plasticizer because it also allowed a greater permeability to water vapor. Peaks at 2Ɵ between 10.00°, 13.81°, 17.67°, 20.0° and 24.34° were observed in films with 12.56 g of starch per 100 g of pulp, which are characteristic of B-starch, due to the presence of long branched chains of amylopectin, with a peak characteristic of lignocellulosic materials. Reflection was more intense at 2Ɵ between 22° for all treatments. The obtained films presented relevant characteristics for the application as edible coating.

A factorial experimental analysis of using wood fly ash as an alkaline activator along with coal fly ash for production of geopolymer-cementitious hybrids.

Alkaline activated materials such as geopolymers and cementitious materials derived from pozzolanic reactions offer several advantages over the currently widely used Portland cement, especially in terms of environmental sustainability and physiochemical properties. However due to the need of an alkaline activator, such as NaOH or KOH, which result in high production cost and requires skilled personnel, they have not been deeply explored and put to use. Here in this study, wood fly ash, a by product of wood combustion is used as an alternative source of alkaline activator for producing such alkaline activated materials along with coal fly ash, where the resulting geopolymer-cementitious hybrid (GCH) was characterized physico-chemically through electron microscopy, BET, FTIR, XRF & XRD. However, the leaching of heavy metals from the wood fly ash could potentially pose an environmental concern. Therefore, the focus of this study is to reduce the leachability factor of wood fly ash involved in the alkaline activated process and to understand the effects of various factors (i.e. water-to-ash ratio (w/a), method of curing, type of alkaline activator and ash sieving) on the leaching process, through factorial experimental analysis. The leaching patterns of various elements such as Pb, Zn, Cr, As. Hg, Se were studied along with the contributing factors and results showed that the dominant factor was the type of alkaline activator (i.e. Wood Fly Ash versus Na2SiO3). By comparing the leaching data to Denmark's leaching criteria, the best performing GCH sample was found to be 0.3DI_p_s (0.3 represents the w/a ratio, "p" denotes that samples were precured and "s" denotes sieving).

The synergistic effect of gamma irradiation and alkaline soaking at low temperature on the pre-deacetylation of α-chitin: Optimization by design of experiment.

The effect of gamma irradiation and alkaline soaking time at low temperature (4 °C) as a pretreatment of α-chitin before its N-deacetylation and the effect temperature, NaOH concentration and the reaction time traditionally used during the deacetylation process were studied by applying a factorial experimental design. The top and bottom levels applied for each factor were 1-25 kGy for γ irradiation dose, 2-18 hours for alkaline soaking time at low temperature (4 °C), 50-85 °C for temperature, 35-60% for NaOH concentration and 30-90 min for reaction time. The measured response of deacetylation degree (DD) was determined by FTIR. The pre-treated samples of α-chitin were characterized by X-ray diffraction, DSC and SEM to investigate physical and chemical modification. The obtained results showed that γ irradiation and alkaline soaking time at low temperature are significant factors. The most influential factor was the temperature during the deacetylation process. The equation of the predictive mathematical model for the DD was obtained as follows: DD(%)=-80.4825+0.4984A[NaOH]+1.1355AT°+0.1505Atime-0.1808ADose+0.9845Asoaktime X-ray diffraction, DSC and SEM revealed that the pre-treatment of α-chitin affected greatly its crystallinity and led to chemical and physical modification of its structure. The pretreatment consisting of γ irradiation and soaking time at 4 °C in alkaline medium played a synergistic effect during the deacetylation process.

Application of Fenton process to remove organic matter and PCBs from waste (fuller's earth) contaminated with insulating oil.

Polychlorinated biphenyls (PCBs) are carcinogenic to humans and can be found in fuller's earth used for the treatment of used transformer oil. This work describes an optimization of the Fenton process for the removal of contaminants from fuller's earth. The effects of pH (2.5 and 4.0), [H2O2] (1.47 and 2.07 mol L-1), and [Fe2+] (1.7 and 40 mmol L-1) were studied. The Fenton process efficiency was monitored using the decreases in the chemical oxygen demand (COD) and the concentrations of oil and grease, total carbon (TC), PCBs, and H2O2. The fuller's earth contaminated with insulating oil presented 35% (w/w) of TC, 34% (w/w) of oil and grease, 297.0 g L-1 COD, and 64 mg of PCBs per kg. The material could therefore be considered a dangerous waste. After Fenton treatment, using a slurry mode, there was a removal of 55% of COD, 20% of oil and grease, and 20% of TC, achieved at pH 2.5 using 2.07 mol L-1 of H2O2 and 40.0 mmol L-1 of Fe2+. No PCBs were detected in the samples after the Fenton treatment, even using smaller amounts of Fenton reagents (1.47 mol L-1 of H2O2, 1.7 mmol L-1 of Fe2+, pH 2.5). The results indicated that the treated fuller's earth was free from PCB residues and could be disposed of in a simple landfill, in accordance with Brazilian PCB regulations.

Modification of Hexachlorobenzene to Molecules with Lower Long-Range Transport Potentials Using 3D-QSAR Models with a Full Factor Experimental Design.

In this study, the hexachlorobenzene molecule was modified by three-dimensional quantitative structure-activity relationship (3D-QSAR) models and a full factor experimental design to obtain new hexachlorobenzene molecules with low migration ability. The 3D-QSAR models (comparative molecular field analysis (CoMFA) and comparative molecular similarity indices analysis (CoMSIA)) were constructed by SYBLY-X 2.0 software, using experimental data of octanol-air partition coefficients (KOA) for 12 chlorobenzenes (CBs) congeners as the dependent variable, and the structural parameters of CBs as independent variables, respectively. A target molecule (hexachlorobenzene; HCB: its long-distance migration capability leads to pollution of the marine environment in Antarctic and Arctic) was modified using the 3D-QSAR contour maps associated with resolution V of the 210-3 full-factorial experimental design method, and 11 modified HCB molecules were produced with a single chlorine atom (-Cl2) and three chlorine atoms (-Cl1, -Cl3, and -Cl5) replaced with electropositive groups (-COOH, -CN, -CF3, -COF, -NO2, -F, -CHF2, -ONO2, and -SiF3) to increase the logKOA. The new molecules had essentially similar biological enrichment functions and toxicities as HCB but were found to be more easily degraded. A 2D-QSAR model and molecular docking technology indicated that both dipole moments and highest occupied orbital energies of the substituents markedly affected migration and degradation of the new molecules. The abilities of the compounds to undergo long distance migration were assessed. The modified HCB molecules (i.e. 2-CN-HCB, 2-CF3-HCB, 1-F-3-COOH-5-NO2-HCB, 1-NO2-3-CN-5-CHF2-HCB and 1-CN-3-F-5-NO2-HCB) moved from a long-range transport potential of the modified molecules to a relatively low mobility class, and the transport potentials of the remaining modified HCB molecules (i.e. 2-COOH-HCB, 2-COF-HCB, 1-COF-3-ONO2-5-NO2-HCB, 1-F-3-CN-5-SiF3-HCB, 1-F-3-COOH-5-SiF3-HCB and 1-CN-3-SiF3-5-ONO2-HCB) also significantly decreased. These results provide a basic theoretical basis for designing environmentally benign molecules based on HCB.

Double or Simple Emulsion Process to Encapsulate Hydrophilic Oxytocin Peptide in PLA-PEG Nanoparticles.

PURPOSE: Oral drug delivery using NPs is a current strategy for poorly absorbed molecules. It offers significant improvement in terms of bioavailability. However, the encapsulation of proteins and peptides in polymeric NPs is a challenge. Firstly, the present study focused on the double emulsion process in order to encapsulate the OXY peptide. Then the technique was challenged by a one-step simplified process, the simple emulsion. METHODS: In order to study the influence of formulation and process parameters, factorial experimental designs were carried on. The responses observed were the NP size (<200 nm in order to penetrate the intestinal mucus layer), the suspension stability (ZP < |30| mV) and the OXY loading. RESULTS: It was thus found that the amount and the nature of surfactant, the ratio between the phases, the amount of PLA-PEG polymer and OXY, the presence of a viscosifying agent, and the duration of the sonication could significantly influence the responses. Finally, OXY-loaded NPs from both processes were obtained with NP size of 195 and 226 nm and OXY loading of 4 and 3.3% for double and simple emulsions, respectively. CONCLUSION: The two processes appeared to be suitable for OXY encapsulation and comparable in term of NP size, peptide drug load and release obtained.

Using factorial experimental design to evaluate the separation of plastics by froth flotation.

This paper proposes the use of factorial experimental design as a standard experimental method in the application of froth flotation to plastic separation instead of the commonly used OVAT method (manipulation of one variable at a time). Furthermore, as is common practice in minerals flotation, the parameters of the kinetic model were used as process responses rather than the recovery of plastics in the separation products. To explain and illustrate the proposed methodology, a set of 32 experimental tests was performed using mixtures of two polymers with approximately the same density, PVC and PS (with mineral charges), with particle size ranging from 2 to 4 mm. The manipulated variables were frother concentration, air flow rate and pH. A three-level full factorial design was conducted. The models establishing the relationships between the manipulated variables and their interactions with the responses (first order kinetic model parameters) were built. The Corrected Akaike Information Criterion was used to select the best fit model and an analysis of variance (ANOVA) was conducted to identify the statistically significant terms of the model. It was shown that froth flotation can be used to efficiently separate PVC from PS with mineral charges by reducing the floatability of PVC, which largely depends on the action of pH. Within the tested interval, this is the factor that most affects the flotation rate constants. The results obtained show that the pure error may be of the same magnitude as the sum of squares of the errors, suggesting that there is significant variability within the same experimental conditions. Thus, special care is needed when evaluating and generalizing the process.

Direct immersion single drop micro-extraction method for multi-class pesticides analysis in mango using GC-MS.

Due the negative effects of pesticides on environment and human health, more efficient and environmentally friendly methods are needed. In this sense, a simple, fast, free from memory effects and economical direct-immersion single drop micro-extraction (SDME) method and GC-MS for multi-class pesticides determination in mango samples was developed. Sample pre-treatment using ultrasound-assisted solvent extraction and factors affecting the SDME procedure (extractant solvent, drop volume, stirring rate, ionic strength, time, pH and temperature) were optimized using factorial experimental design. This method presented high sensitive (LOD: 0.14-169.20µgkg-1), acceptable precision (RSD: 0.7-19.1%), satisfactory recovery (69-119%) and high enrichment factors (20-722). Several obtained LOQs are below the MRLs established by the European Commission; therefore, the method could be applied for pesticides determination in routing analysis and custom laboratories. Moreover, this method has shown to be suitable for determination of some of the studied pesticides in lime, melon, papaya, banana, tomato, and lettuce.

Effects analysis of substituent characteristics and solvents on the photodegradation of polybrominated diphenyl ethers.

The ultraviolet spectra and electron transition information of 209 polybrominated diphenyl ethers (PBDEs) in gas were first calculated via time-dependent density functional theory using Gaussian 09 software. The main and second-order interactional effects of substituent characteristics on the photodegradation of PBDEs were then analysed using a full factorial experimental design. Solvent effects were considered to research the effect and promotion mechanism of solvent molecules on the photodegradation of PBDEs compared with that in gas. The results showed that the introduction of substituents at each position promoted excitation of PBDEs from their ground states to excited states to induce photodegradation. The different positions affected the photodegradation of PBDEs with magnitudes of para > meta > ortho. The congeners with a concentrated distribution of substituents can always be photodegraded more easily than those with separated substituents. From the viewpoint of light-induced reactions, the electron transfer reactions between molecules of PBDE* T1 and Solvent* T1 are the main driving force for the enhanced photodegradation of PBDEs in solvents compared with that in gas.

Effect analysis of quantum chemical descriptors and substituent characteristics on Henry's law constants of polybrominated diphenyl ethers at different temperatures.

Twelve substituent descriptors, 17 quantum chemical descriptors and 1/T were selected to establish a quantitative structure-property relationship (QSPR) model of Henry's law constants for 7 polybrominated diphenyl ethers (PBDEs) at five different temperatures. Then, the lgH of 202 congeners at different temperatures were predicted. The variation rule and regulating mechanism of lgH was studied from the perspectives of both quantum chemical descriptors and substituent characteristics. The R2 for modeling and testing sets of the final QSPR model are 0.977 and 0.979, respectively, thus indicating good fitness and predictive ability for Henry' law constants of PBDEs at different temperatures. The favorable hydrogen binding sites are the 5,5',6,6'-positions for high substituent congeners and the O atom of the ether bond for low substituent congeners, which affects the interaction between PBDEs and water molecules. lgH is negatively and linearly correlated with 1/T, and the variation trends of lgH with temperature are primarily regulated by individual substituent characteristics, wherein: the more substituents involved, the smaller the lgH. The significant sequence for the main effect of substituent positions is para>meta>ortho, where the ortho-positions are mainly involved in second-order interaction effect (64.01%). Having two substituents in the same ring also provides a significant effect, with 81.36% of second-order interaction effects, particularly where there is an adjacent distribution (55.02%).

Quality by design (QbD), Process Analytical Technology (PAT), and design of experiment applied to the development of multifunctional sunscreens.

Multifunctional formulations are of great importance to ensure better skin protection from harm caused by ultraviolet radiation (UV). Despite the advantages of Quality by Design and Process Analytical Technology approaches to the development and optimization of new products, we found in the literature only a few studies concerning their applications in cosmetic product industry. Thus, in this research work, we applied the QbD and PAT approaches to the development of multifunctional sunscreens containing bemotrizinol, ethylhexyl triazone, and ferulic acid. In addition, UV transmittance method was applied to assess qualitative and quantitative critical quality attributes of sunscreens using chemometrics analyses. Linear discriminant analysis allowed classifying unknown formulations, which is useful for investigation of counterfeit and adulteration. Simultaneous quantification of ethylhexyl triazone, bemotrizinol, and ferulic acid presented at the formulations was performed using PLS regression. This design allowed us to verify the compounds in isolation and in combination and to prove that the antioxidant action of ferulic acid as well as the sunscreen actions, since the presence of this component increased 90% of antioxidant activity in vitro.

Effects of Fumed Silica and Draw Ratio on Nanocomposite Polypropylene Fibers.

Hydrophylic fumed silica AR974 was tested as a potential nanofiller for the production of composite isotactic polypropylene filaments/fibers (containing 0.25⁻2 vol % of nanoparticles) via melt compounding and subsequent hot drawing. The objectives of this study were as follows: (i) to investigate the effects of the composition and the processing conditions on the microstructure and the thermal and mechanical properties of the produced fibers; (ii) to separate the effects of silica addition from those produced by fiber drawing; and (iii) to interpret the changes in the matrix molecular mobility (produced by silica and/or drawing). Scanning electron microscopy (SEM) evidenced a good dispersion of nanoparticles at fractions up to 0.5 vol % of the nanofiller. X-ray diffraction (XRD) analyses revealed the increase in crystallinity after drawing of both neat polypropylene (PP) and produced nanocomposite fibers. Consequently, tensile modulus and stress at break of the fibers were enhanced. Drawn fibers containing 0.25⁻0.5 vol % of nanofiller showed also a remarkable increase in the creep resistance. Loss modulus of drawn fibers showed a pronounced α-relaxation peak at about 65 °C; the higher the draw ratio, the higher the peak intensity. Thermal and mechanical properties of composite fibers were improved due to the combined effects of nanofiller reinforcement and fiber orientation produced during hot drawing. Both fumed silica and draw ratio were significantly effective on tensile modulus and tenacity of nanocomposite fibers up to 0.5 vol % of AR974.

Analysis of positions and substituents on genotoxicity of fluoroquinolones with quantitative structure-activity relationship and 3D Pharmacophore model.

The genotoxicity values of 21 quinolones were studied to establish a quantitative structure-activity relationship model and 3D Pharmacophore model separately for screening essential positions and substituents that contribute to genotoxicity of fluoroquinolones (FQs). A full factor experimental design was performed to analyze the specific main effect and second-order interaction effect of different positions and substituents on genotoxicity, forming a reasonable modification scheme which was validated on typical FQ with genotoxicity and efficacy data. Four positions (1, 5, 7, 8) were screened finally to form the full factorial experimental design which contained 72 congeners in total, illustrating that: the dominant effect of 5 and 7-positions on genotoxicity of FQs is main effect; meanwhile the effect of 1 and 8-positions is a second-order interaction effect; two adjacent positions always have stronger second-order interaction effect and lower genotoxicity; the obtained modification scheme had been validated on typical FQ congeners with the modified compound has a lower genotoxicity, higher synthesis feasibilities and efficacy.

Optimization of Cadmium (CD(2+)) removal from aqueous solutions by novel biosorbent.

In this research, dead leaves of a common ornamental plant, Dracaena draca known also as dragon tree was used as a biosorbent for the removal of Cadmium (Cd(2+)) from aqueous solutions using a full 2(3) factorial experimental design. Three factors were investigated at two different levels, metal ion concentration (X = 10 and 100 ppm), hydrogen ion concentration (Ph = 2 and 7) and biomass dose (BD = 0.1 and 0.5g). Experiments were carried out in duplicates with 50 ml of Cd(2+) solutions at room temperature. When comparing observed values (experimental) with calculated values (model), they were set closely together that allowed suggesting a normal distribution where (R(2) = 0.9938). A characterization of the biosorbent was done by pHzpc and SEM-EDAX. Results also showed that the most significant effect for Cd(2+) biosorption was ascribed to (X). The interaction effects of (pH BD) and (X pH) were found to have significant influence on Cd(2+) removal efficiency. The highest Cd(2+) removal percentage attained by 79.60% at X = 10 ppm, pH = 7 and BD = 0.5g. The reusability of the biosorbent was tested in three desorption cycles and the regeneration efficiency was above 99.7%.

Extraction of tetracyclinic antibiotic residues from fish filet: comparison and optimization of different procedures using liquid chromatography with fluorescence detection.

Anti-microbials have been used to control the quality of the aquatic environment for both prophylactic and therapeutic purposes. Tetracyclines are among the main antimicrobials used in aquaculture, and present a particular difficulty for extraction, due to a complex structure and high interaction with components of the biological matrix. In this study, different techniques of extraction and clean-up of antimicrobials of the tetracycline class in tilapia filets have been optimized and compared, followed by validation of the methodology using the best procedure. Oxytetracycline, doxycycline, tetracycline and chlortetracycline were analyzed by HPLC-fluorescence under the following conditions: organic mobile phase composed of methanol:acetonitrile (1:1, v/v) and aqueous mobile phase containing sodium acetate (0.0375molL(-1)), calcium chloride (0.0175molL(-1)) and EDTA (0.0125molL(-1)) at pH 7.00. The chromatographic analysis was performed using a mobile phase gradient with a flow rate of 1mLmin(-1) and detection wavelength of 385/528nm (λexc/λem). Four extraction methods have been evaluated, namely: liquid-liquid partition; solid phase extraction (SPE) using phenyl, C18 and polymeric Oasis-HLB stationary phases; dispersive SPE (dSPE) using polymeric adsorbent XAD 16 resin; and QuEChERS. The methods have been optimized with fractional factorial experimental design and compared by the extraction efficiency. The liquid-liquid extraction and the QuEChERS methods showed low extraction efficiencies (14-30%) for the analytes. The use of dSPE showed good efficiency (40-60%), but with low precision and high consumption of time. Among the evaluated extraction techniques the use of SPE showed the best results, with emphasis on the phenyl phase (58-76%), and has been validated for analysis of residues of tetracyclines in tilapia muscle regarding selectivity, linearity, precision and limits of detection and quantification. The validated method was adequate for the investigation of the analytes at residue levels.