Functionalized magnetic lipase/Cu3(PO4)2 hybrid nanoflower: Synthesis, characterization, and enzymatic evaluation.

This paper reports the synthesis of magnetic lipase/Cu3(PO4)2 hybrid nanoflowers via a rapid ultrasonication method. The enzyme immobilization and nanoflower growth mechanism can be described as the (a) Fe2+, Cu2+, and phosphate "binding", (b) metal phosphate crystals formation, (c) formation and growth of metal phosphate crystals to form plate-like structures, and (d) self-assembly of plate structures that forms a flower-like structure. Some factors contributing to the morphology of the hybrid nanoflowers structure includes the time and concentration of lipase were studied. The effect of temperature, pH, and duration on the enzyme immobilization yield were also studied. In addition, the strong magnetic property (9.73 emu g-1) of the nanoflowers resulted in higher retrievability and reusability after repeated usage. Furthermore, the catalytic activity of lipase/Cu3(PO4)2 hybrid nanoflowers was investigated and the ideal conditions were determined whereby, the maximum activity was calculated to be 1511 ± 44 U g-1, showing a catalytic enhancement of 89% in comparison to free lipase. The reusability study showed that, after 5 cycles, the magnetic lipase/Cu3(PO4)2 nanoflowers successfully retained 60% of its initial activity. From the results obtained, it is worth noting that, the magnetic lipase/Cu3(PO4)2 hybrid nanoflowers are highly efficient in industrial biocatalytic applications.

Niosomes in cancer treatment: A focus on curcumin encapsulation.

Curcumin is widely used as a therapeutic drug for cancer treatment. However, its limited absorption and rapid excretion are the major therapeutic limitations to its clinical use. Using niosomes as a curcumin delivery system is a cheap, easy, and less toxic strategy for enhancing the absorption of curcumin by cells and delaying its excretion. Thus, there is a vital need to explore curcumin niosomes to configure the curcumin to suitably serve and aid current pharmacokinetics in treatments for cancer. To date, no comprehensive review has focused on the cytotoxic effects of curcumin niosomes on malignant cells. Thus, this review provides a critical analysis of the curcumin niosomes in cancer treatment, formulations of curcumin niosomes, characterizations of curcumin niosomes, and factors influencing their performance. The findings from this review article can strongly accelerate the understanding of curcumin niosomes and pave a brighter direction towards advances in the pharmaceutical, biotechnology, and medical industries.

Dataset of ultrasound-assisted extraction of anthocyanin from the petals of Clitoria ternatea using Taguchi method and effect of storage conditions on the anthocyanin stability.

Anthocyanins are natural water-soluble colourants with a number of reported health benefits and are an excellent alternative to artificial dyes. Anthocyanins from Clitoria ternatea were obtained using ultrasound-assisted extraction with glycerol-water (60:40 w/v). The anthocyanins in the extract were measured at wavelength 550 and 700 nm using a UV-visible spectrophotometer and expressed in terms of total anthocyanins content (TAC). Taguchi method was employed to optimize the extraction parameters that include the extraction time (30 to 50 min), extraction temperature (40 to 60 °C), and solvent to solid ratio (10:1 to 30:1), with TAC as the response. The obtained data showed the optimum extraction parameters as 30 min extraction time, 50 °C extraction temperature, and 10:1 solvent to solid ratio. The anthocyanin's storage stability was analyzed for 7 days at varying storage temperatures and exposure to light. The present dataset in this article indicated the glycerol-water system as a green alternative for anthocyanin extraction and acted as a storage medium. Furthermore, our methodology can be applied to optimize the anthocyanins extraction process, manipulate storage conditions and improve the extract quality.

Choline Chloride-urea Deep Eutectic Mixture Water for the Synthesis of an Amphiphilic Compound of Glyceryl Monocaffeate.

The Lipase-catalyzed synthesis of glyceryl monocaffeate (GMC) in choline chloride-urea of natural deep eutectic solvent (NADES) media is reported to provide amphiphilic character to caffeic acid (CA). The modification of CA into GMC could potentially increase its solubility and widen the application of CA's biological activities in water and oil-based systems. The high conversion was achieved when the reaction was carried out with the addition of more than 20 %v/v water, at a high molar ratio of glycerol and 40°C. It was found that the lipase-catalyzed transesterification of ethyl caffeate (EC) and glycerol in choline chloride-urea of DES media obeyed ping-pong bi-bi mechanism with Vmax = 10.9 mmol.min-1, KmEC = 126.5 mmol and KmGly = 1842.7 mmol.

Fast liquid chromatography for racemic atenolol acetate separation-The analytical protocol.

Kinetic resolution of (R,S)-atenolol is a faster strategy to produce (S)-atenolol. Since this racemate is a less soluble compound, resolution of its ester offers high concentrations in the process. A good analytical method is required to observe the enantiomer concentrations. This paper described application of ultra-fast liquid chromatography on the atenolol ester separation using different resolution media and analytical procedures. Chiralcel OD column resolved the ester. The chromatograms indicated different characteristics of the process. The enantiomers could be recognized by the column in less than 1 (one) hour. Symmetrical peaks were obtained, but several procedures produced peaks with wide bases and slanted baselines. Efficient enantioresolution was obtained at high mobile phase flow rate, decreased concentration of amine-type modifier, but increased alcohol content in the mobile phase. High UV detection wavelength was required. At 1.0 mL/min, the (90/10/0.5) composition resulted α = 1.46 and RS  = 0.9998 that were good separation.

Factors screening to statistical experimental design of racemic atenolol kinetic resolution via transesterification reaction in organic solvent using free Pseudomonas fluorescens lipase.

As the (R)-enantiomer of racemic atenolol has no ß-blocking activity and no lack of side effects, switching from the racemate to the (S)-atenolol is more favorable. Transesterification of racemic atenolol using free enzymes investigated as a resource to resolve the racemate via this method is limited. Screenings of enzyme, medium, and acetyl donor were conducted first to give Pseudomonas fluorescens lipase, tetrahydrofuran, and vinyl acetate. A statistical design of the experiment was then developed using Central Composite Design on some operational factors, which resulted in the conversions of 11.70-61.91% and substrate enantiomeric excess (ee) of 7.31-100%. The quadratic models are acceptable with R2 of 95.13% (conversion) and 89.63% (ee). The predicted values match the observed values reasonably well. Temperature, agitation speed, and substrate molar ratio factor have low effects on conversion and ee, but enzyme loading affects the responses highly. The interaction of temperature-agitation speed and temperature-substrate molar ratio show significant effects on conversion, while temperature-agitation speed, temperature-substrate molar ratio, and agitation speed-substrate molar ratio affect ee highly. Optimum conditions for the use of Pseudomonas fluorescens lipase, tetrahydrofuran, and vinyl acetate were found at 45°C, 175 rpm, 2000 U, and 1:3.6 substrate molar ratio.

Chromatographic comparison of atenolol separation in reaction media on cellulose tris-(3,5-dimethylphenylcarbamate) chiral stationary phase using ultra fast liquid chromatography.

Because chiral liquid chromatography (LC) could become a powerful tool to estimate racemic atenolol quantity, excellent enantiomeric separation should be produced during data acquisition for satisfactory observation of atenolol concentrations throughout the racemic resolution processes. Selection of chiral LC column and analytical protocol that fulfill demands of the ultra fast LC analysis is essential. This article describes the characteristics of atenolol chromatographic separation that resulted from different resolution media and analytical protocols with the use of a Chiralcel® OD column. The chromatograms showed quite different characteristics of the separation process. The single enantiomer and racemic atenolol could be recognized by the Chiralcel® OD column in less than 20 min. Symmetrical peaks were obtained; however, several protocols produced peaks with wide bases and slanted baselines. Observations showed that efficient enantioresolution of racemic atenolol was obtained at slow mobile phase flow rate, decreased concentration of amine-type modifier but increased alcohol content in mobile phase and highest ultraviolet detection wavelength were required. The optimal ultra fast LC protocol enables to reduce and eliminate the peaks of either the atenolol solvent or the buffers and provided the highest peak intensities of both atenolol enantiomers.

Sorption of SO(2) and NO from simulated flue gas over rice husk ash (RHA)/CaO/CeO(2) sorbent: evaluation of deactivation kinetic parameters.

In this study, the kinetic parameters of rice husk ash (RHA)/CaO/CeO(2) sorbent for SO(2) and NO sorptions were investigated in a laboratory-scale stainless steel fixed-bed reactor. Data experiments were obtained from our previous results and additional independent experiments were carried out at different conditions. The initial sorption rate constant (k(0)) and deactivation rate constant (k(d)) for SO(2)/NO sorptions were obtained from the nonlinear regression analysis of the experimental breakthrough data using deactivation kinetic model. Both the initial sorption rate constants and deactivation rate constants increased with increasing temperature, except at operating temperature of 170 °C. The activation energy and frequency factor for the SO(2) sorption were found to be 18.0 kJ/mol and 7.37 × 10(5)cm(3)/(g min), respectively. Whereas the activation energy and frequency factor for the NO sorption, were estimated to be 5.64 kJ/mol and 2.19 × 10(4)cm(3)/(g min), respectively. The deactivation kinetic model was found to give a very good agreement with the experimental data of the SO(2)/NO sorptions.

The feasibility study of crude palm oil transesterification at 30 °C operation.

The objective of this research is to investigate the potential of transesterification of crude palm oil (CPO) to biodiesel at 30 degrees C. The mass transfer limitations problem crucial at 30 degrees C due to the viscosity of CPO has been addressed. The process parameters that are closely related to mass transfer effects like enzyme loading, agitation speed and reaction time were optimized. An optimum methanol to oil substrate molar ratio at 6.5:1 was observed and maintained throughout the experiments. The optimum operating condition for the transesterification process was found at 6.67 wt% of enzyme loading and at 150 rpm of agitation speed. The corresponding initial reaction and FAME yield obtained at 6 h were 89.29% FAME yield/hr and 85.01%, respectively. The 85% FAME yield obtained at 30 degrees C operation of CPO transesterification shows that the process is potentially feasible for the biodiesel synthesis.

Reactive extraction of Jatropha curcas L. seed for production of biodiesel: process optimization study.

Biodiesel from Jatropha curcas L. seed is conventionally produced via a two-step method: extraction of oil and subsequent esterification/transesterification to fatty acid methyl esters (FAME), commonly known as biodiesel. Contrarily, in this study, a single step in situ extraction, esterification and transesterification (collectively known as reactive extraction) of J. curcas L. seed to biodiesel, was investigated and optimized. Design of experiments (DOE) was used to study the effect of various process parameters on the yield of FAME. The process parameters studied include reaction temperature (30-60 degrees C), methanol to seed ratio (5-20 mL/g), catalyst loading (5-30 wt %), and reaction time (1-24 h). The optimum reaction condition was then obtained by using response surface methodology (RSM) coupled with central composite design (CCD). Results showed that an optimum biodiesel yield of 98.1% can be obtained under the following reaction conditions: reaction temperature of 60 degrees C, methanol to seed ratio of 10.5 mL/g, 21.8 wt % of H(2)SO(4), and reaction period of 10 h.

Thermodynamics and inhibition studies of lipozyme TL IM in biodiesel production via enzymatic transesterification.

In order to characterize enzyme activity and stability corresponding to temperature effects, thermodynamic studies on commercial immobilized lipase have been carried out via enzymatic transesterification. An optimum temperature of 40 degrees C was obtained in the reaction. The decreasing reaction rates beyond the optimum temperature indicated the occurrence of reversible enzyme deactivation. Thermodynamic studies on lipase denaturation exhibited a first-order kinetics pattern, with considerable stability through time shown by the lipase as well. The activation and deactivation energies were 22.15 kJ mol(-1) and 45.18 kJ mol(-1), respectively, implying more energy was required for the irreversible denaturation of the enzyme to occur. At water content of 0.42%, the initial reaction rate and FAME yield displayed optimum values of 3.317 g/L min and 98%, respectively.

Parameters optimization of rice husk ash (RHA)/CaO/CeO2 sorbent for predicting SO2/NO sorption capacity using response surface and neural network models.

In this work, the application of response surface and neural network models in predicting and optimizing the preparation variables of RHA/CaO/CeO(2) sorbent towards SO(2)/NO sorption capacity was investigated. The sorbents were prepared according to central composite design (CCD) with four independent variables (i.e. hydration period, RHA/CaO ratio, CeO(2) loading and the use of RHA(raw) or pretreated RHA(600 degrees C) as the starting material). Among all the variables studied, the amount of CeO(2) loading had the largest effect. The response surface models developed from CCD was effective in providing a highly accurate prediction for SO(2) and NO sorption capacities within the range of the sorbent preparation variables studied. The prediction of CCD experiment was verified by neural network models which gave almost similar results to those determined by response surface models. The response surface models together with neural network models were then successfully used to locate and validate the optimum hydration process variables for maximizing the SO(2)/NO sorption capacities. Through this optimization process, it was found that maximum SO(2) and NO sorption capacities of 44.34 and 3.51 mg/g, respectively could be obtained by using RHA/CaO/CeO(2) sorbents prepared from RHA(raw) with hydration period of 12h, RHA/CaO ratio of 2.33 and CeO(2) loading of 8.95%.

Selection of metal oxides in the preparation of rice husk ash (RHA)/CaO sorbent for simultaneous SO2 and NO removal.

In this work, the removal of SO(2) and NO from simulated flue gas from combustion process was investigated in a fixed-bed reactor using rice husk ash (RHA)/CaO-based sorbent. Various metal precursors were used in order to select the best metal impregnated over RHA/CaO sorbents. The results showed that RHA/CaO sorbents impregnated with CeO(2) had the highest sorption capacity among other impregnated metal oxides for the simultaneous removal of SO(2) and NO. Infrared spectroscopic results indicated the formation of both sulfate (SO(4)(2-)) and nitrate (NO(3)(-)) species due to the catalytic role played by CeO(2). Apart from that, the catalytic activity of the RHA/CaO/CeO(2) sorbent was found to be closely related to its physical properties (specific surface area, total pore volume and average pore diameter).

Continuous biosynthesis of biodiesel from waste cooking palm oil in a packed bed reactor: optimization using response surface methodology (RSM) and mass transfer studies.

This study aimed to develop an optimal continuous procedure of lipase-catalyzes transesterification of waste cooking palm oil in a packed bed reactor to investigate the possibility of large scale production further. Response surface methodology (RSM) based on central composite rotatable design (CCRD) was used to optimize the two important reaction variables packed bed height (cm) and substrate flow rate(ml/min) for the transesterification of waste cooking palm oil in a continuous packed bed reactor. The optimum condition for the transesterification of waste cooking palm oil was as follows: 10.53 cm packed bed height and 0.57 ml/min substrate flow rate. The optimum predicted fatty acid methyl ester (FAME) yield was 80.3% and the actual value was 79%. The above results shows that the RSM study based on CCRD is adaptable for FAME yield studied for the current transesterification system. The effect of mass transfer in the packed bed reactor has also been studied. Models for FAME yield have been developed for cases of reaction control and mass transfer control. The results showed very good agreement compatibility between mass transfer model and the experimental results obtained from immobilized lipase packed bed reactor operation, showing that in this case the FAME yield was mass transfer controlled.

Chemoenzymatic and microbial dynamic kinetic resolutions.

This review tracks a decade of dynamic kinetic resolution developments with a biocatalytic inclination using enzymatic/microbial means for the resolution part followed by the racemization reactions either by means of enzymatic or chemocatalyst. These fast developments are due to the ability of the biocatalysts to significantly reduce the number of synthetic steps which are common for conventional synthesis. Future developments in novel reactions and products of dynamic kinetic resolutions should consider factors that are needed to be extracted at the early synthetic stage to avoid inhibition at scale-up stage have been highlighted.

Evaluation of various additives on the preparation of rice husk ash (RHA)/CaO-based sorbent for flue gas desulfurization (FGD) at low temperature.

This paper examines the effectiveness of 10 additives toward improving SO2 sorption capacities (SSC) of rice husk ash (RHA)/lime (CaO) sorbent. The additives examined are NaOH, CaCl2, LiCl, NaHCO3, NaBr, BaCl2, KOH, K2HPO4, FeCl3 and MgCl2. Most of the additives tested increased the SSC of RHA/CaO sorbent, whereby NaOH gave highest SSC (30mg SO2/g sorbent) at optimum concentration (0.25mol/l) compared to other additives examined. The SSC of RHA/CaO sorbent prepared with NaOH addition was also increases from 17.2 to 39.5mg SO2/g sorbent as the water vapor increases from 0% RH to 80% RH. This is probably due to the fact that most of additives tested act as deliquescent material, and its existence increases the amount of water collected on the surface of the sorbent, which played an important role in the reaction between the dry-type sorbent and SO2. Although most of the additives were shown to have positive effect on the SSC of the RHA/CaO sorbent, some were found to have negative or insignificant effect. Thus, this study demonstrates that proper selection of additives can improve the SSC of RHA/CaO sorbent significantly.

5-Chloro-8-hydr-oxy-6-methyl-1,4-naphthoquinone.

The mol-ecule of the title compound, C(11)H(7)ClO(3), is planar, with a maximum deviation of 0.0383 (10) Šfrom the naphthoquinone plane. An intra-molecular O-H⋯O hydrogen bond generates an S(6) ring motif. The crystal packing is stabilized by inter-molecular C-H⋯O hydrogen bonds. Short intra-molecular Cl⋯O [2.8234 (8) Å] and O⋯O [2.5530 (11) Å], and inter-molecular Cl⋯Cl [3.2777 (3) Å] contacts further stabilize the crystal structure.

Enantioseparation of (R,S)-ketoprofen using Candida antarctica lipase B in an enzymatic membrane reactor.

An enzymatic membrane reactor (EMR) for enantioseparation of (R,S)-ketoprofen via Candida antarctica lipase B (CALB) as biocatalyst was investigated. A comparative study of free and immobilized CALB was further conducted. The catalytic behaviour of CALB in an EMR was affected by the process parameters of enzyme load, substrate concentration, substrate molar ratio, lipase solution pH, reaction temperature, and substrate flow rate. Immobilization of CALB in the EMR was able to reduce the amount of enzyme required for the enantioseparation of (R,S)-ketoprofen. Immobilized CALB in the EMR assured higher reaction capacity, better thermal stability, and reusability. It was also found to be more cost effective and practical than free CALB in a batch reactor.

Analysis of SO2 sorption capacity of rice husk ash (RHA)/CaO/NaOH sorbents using response surface methodology (RSM): untreated and pretreated RHA.

The SO2 sorption capacity (SSC) of sorbents prepared from rice husk ash (RHA) with NaOH as additive was studied in a fixed-bed reactor. The sorbents were prepared using a water hydration method by slurrying RHA, CaO, and NaOH. Response surface methodology (RSM) based on four-variable central composite face centered design (CCFCD) was employed in the synthesis of the sorbents. The correlation between the sorbent SSC (as response) with four independent sorbent preparation variables, i.e. hydration period, RHA/CaO ratio, NaOH amount, and drying temperature, were presented as empirical mathematical models. Among all the variables studied, the amount of NaOH used was found to be the most significant variable affecting the SSC of the sorbents prepared. The SSC for sorbent prepared with the addition of NaOH was found to be significantly higher than sorbents prepared without NaOH. This is probably because NaOH is a deliquescent material, and its existence increases the amount of water collected on the surface of the sorbent, a condition required for sorbent-SO2 reaction to occur at low temperature. The effect of further treatment of RHA at 600 degrees C was also investigated. Although pretreated RHA sorbents demonstrated higher SSC as compared to untreated RHA sorbents, nevertheless, at optimum conditions, sorbents prepared from untreated RHA was found to be more favorable due to practical and economic concerns.

5-Hydr-oxy-8-nitro-1,4-naphthoquinone.

The title compound, C(10)H(5)NO(5), features an intra-molecular O-H⋯O hydrogen bond, forming a six-membered ring with an S(6) ring motif. The nitro group makes a dihedral angle of 71.66 (5)° with the plane of the benzene ring to which it is bound. The two rings are almost coplanar, with a dihedral angle of 4.44 (5)°. Short inter-molecular distances between the centroids of the six-membered rings [3.7188 (6)-3.8299 (6) Å] indicate the existence of π-π inter-actions. The inter-esting features of the crystal structure are the short inter-molecular O⋯O and O⋯N inter-actions. The crystal packing is stabilized by intra-molecular O-H⋯O and inter-molecular C-H⋯O (×3) hydrogen bonds, and C-H⋯π inter-actions.