Response surface methodology (RSM) to evaluate both the extraction of triterpenes and sterols from jackfruit seed with supercritical CO2 and the biological activity of the extracts.

Jackfruit seeds are an underestimate residue having important biological activity such as anti-inflammatory, cytotoxicity and antimicrobial effects. However few researches have been done for this material using alternative extraction technologies, so this study aimed to evaluate the extraction of triterpenes and sterols from jackfruit seed by applying high- and low-pressure techniques. Response surface methodology (RSM) was used to determine the best conditions of pressure, temperature and CO2 flow rate for extraction with supercritical CO2. The yield and profile of these compounds were compared with the low pressure technique, which was considered as a reference. In vitro biological tests of anti-inflammatory activity and cytotoxicity in L929 and RAW 264.7 cells were also performed. The best extraction conditions in SFE for sterols were 40 °C/20 MPa/4 mL min-1 (0.832 ± 0.007 mgSR g-1 sample) and 40 °C/20 MPa/3 mL min-1 (0.800 ± 0.009 mgSR g-1 sample), for triterpenes were 50 °C/12 MPa/4 mL min-1 (1.501 ± 0.004 mgTT g-1 sample) and 45 °C/9.3 MPa/3.5 mL min-1 (1.485 ± 0.004 mgTT g-1 sample). No cytotoxic activity was detected in L929 cells in the extracts obtained from ethanol up to concentration of 100 µg mL-1 of extract. The Pearson's coefficient indicated that the reduction in cell viability was related to the concentration of triterpenes. Anti-inflammatory assays showed that some extracts could inhibit the inflammatory action induced in RAW 264.7 cells at concentration of 30 µg mL-1 of extract. Our results justify the further exploration of these characteristics to obtain natural products for the pharmaceutical and food industries.

Dissolution of adhesive resins present in plastic waste to recover polyolefin by sink-float separation processes.

This study investigated the dissolution of adhesive resins present in polyolefin films that cause plastic materials to adhere to each other. The process of dissolution was made by the use of ethyl acetate and followed by separation through the sink-float process. The objective was to separate and characterize polyolefin films from plastic solid waste derived from recycled post-consumer paper. Through these procedures, 6% polyethylene of high-density (HDPE), 14% polyethylene of low-density (LDPE) and 39% polypropylene (PP) were separated and recovered from plastic waste. Fourier transform infrared spectroscopy (FTIR), thermal gravimetric analyzes (TGA), differential scanning calorimetry (DSC), and dynamic mechanical analysis (DMA) were conducted to determine the chemical, thermal and mechanical properties of the recovered polymers and to establish a comparison with standard commercial polymers. It demonstrated that recovered material kept their chemical, thermal, and mechanical properties. This process indicates possible economic viability considering the demand, the market value of the PP, and the required investment to be implemented in the recycling process that could be amortized in a short period of time. Moreover, the organic solvent used in the dissolution process can be easily recovered by distillation.

Robust estimation of thermodynamic parameters (ΔH, ΔS and ΔCp) for prediction of retention time in gas chromatography - Part I (Theoretical).

An approach that is commonly used for calculating the retention time of a compound in GC departs from the thermodynamic properties ΔH, ΔS and ΔCp of phase change (from mobile to stationary). Such properties can be estimated by using experimental retention time data, which results in a non-linear regression problem for non-isothermal temperature programs. As shown in this work, the surface of the objective function (approximation error criterion) on the basis of thermodynamic parameters can be divided into three clearly defined regions, and solely in one of them there is a possibility for the global optimum to be found. The main contribution of this study was the development of an algorithm that distinguishes the different regions of the error surface and its use in the robust initialization of the estimation of parameters ΔH, ΔS and ΔCp.

Robust estimation of thermodynamic parameters (ΔH, ΔS and ΔCp) for prediction of retention time in gas chromatography - Part II (Application).

For this work, an analysis of parameter estimation for the retention factor in GC model was performed, considering two different criteria: sum of square error, and maximum error in absolute value; relevant statistics are described for each case. The main contribution of this work is the implementation of an initialization scheme (specialized) for the estimated parameters, which features fast convergence (low computational time) and is based on knowledge of the surface of the error criterion. In an application to a series of alkanes, specialized initialization resulted in significant reduction to the number of evaluations of the objective function (reducing computational time) in the parameter estimation. The obtained reduction happened between one and two orders of magnitude, compared with the simple random initialization.

Fast and accurate numerical method for predicting gas chromatography retention time.

Predictive modeling for gas chromatography compound retention depends on the retention factor (ki) and on the flow of the mobile phase. Thus, different approaches for determining an analyte ki in column chromatography have been developed. The main one is based on the thermodynamic properties of the component and on the characteristics of the stationary phase. These models can be used to estimate the parameters and to optimize the programming of temperatures, in gas chromatography, for the separation of compounds. Different authors have proposed the use of numerical methods for solving these models, but these methods demand greater computational time. Hence, a new method for solving the predictive modeling of analyte retention time is presented. This algorithm is an alternative to traditional methods because it transforms its attainments into root determination problems within defined intervals. The proposed approach allows for tr calculation, with accuracy determined by the user of the methods, and significant reductions in computational time; it can also be used to evaluate the performance of other prediction methods.