Synthesis of Biodiesel from Canola Oil Using Heterogeneous Base Catalyst

A series of alkali metal (Li, Na, K) promoted alkali earth oxides (CaO, BaO, MgO), as well as K₂CO₃ supported on alumina (Al₂O₃), were prepared and used as catalysts for transesterification of canola oil with methanol. Four catalysts such as K₂CO₃/Al₂O₃ and alkali metal (Li, Na, K) promoted BaO were effective for transesterification with >85 wt% of methyl esters. ICP-MS analysis revealed that leaching of barium in ester phase was too high (~1,000 ppm) when BaO based catalysts were used. As barium is highly toxic, these catalysts were not used further for transesterification of canola oil. Optimization of reaction conditions such as molar ratio of alcohol to oil (6:1–12:1), reaction temperature (40–60 °C) and catalyst loading (1–3 wt%) was performed for most efficient and environmentally friendly K₂CO₃/Al₂O₃ catalyst to maximize ester yield using response surface methodology (RSM). The RSM suggested that a molar ratio of alcohol to oil 11.48:1, a reaction temperature of 60 °C, and catalyst loading 3.16 wt% were optimum for the production of ester from canola oil. The predicted value of ester yield was 96.3 wt% in 2 h, which was in agreement with the experimental results within 1.28%.     

Identification of In Vitro Metabolites of Synthetic Phenolic Antioxidants BHT,BHA, and TBHQ by LC-HRMS/MS

Butylated hydroxytoluene (BHT) and its analogs, butylated hydroxyanisole (BHA) and tert-butyl-hydroquinone (TBHQ), are widely used synthetic preservatives to inhibit lipid oxidation in the food, cosmetic and pharmaceutical industries. Despite their widespread use, little is known about their human exposure and related biotransformation products. The metabolism of these compounds was investigated using in vitro incubations with human and rat liver fractions. Liquid chromatography coupled to high-resolution tandem mass spectrometry was employed to detect and characterize stable and reactive species formed via oxidative metabolism, as well as phase II conjugates. Several oxidative metabolites have been detected, as well as glutathione, glucuronide, and sulfate conjugates, many of which were not previously reported. A combination of accurate mass measurements, MS/MS fragmentation behavior, and isotope-labeling studies were used to elucidate metabolite structures.     

Radiological risk analysis of particle accelerators

Considering the growing use of high-current accelerators in medicine, industry and research, there is a need for evaluating the hazard potentials of new accelerator systems from the design stage itself. The present paper discusses the factors taken care of in a radiological safety analysis of accelerators. Possible hazards identified are beam loss, target rupture, faulty components and personnel being trapped in an active area. Human error is one of the major factors leading to accelerator hazard. How radiation dose to both occupational workers and general public is reduced and taken care of are discussed.     

Toxin screening in phytoplankton: detection and quantitation using MALDI triple quadrupole mass spectrometry

The investigation of a MALDI triple quadrupole instrument for the analysis of spirolide toxins in phytoplankton samples is described in this study. A high-frequency (kHz) laser was employed for MALDI, generating a semicontinuous ion beam, thus taking advantage of the high duty cycle obtained in sensitive triple quadrupole MRM experiments. Initially, several experimental parameters such as type of organic matrix and concentration, solvent composition, and matrix-to-analyte ratio were optimized, and their impact on sensitivity and precision of the obtained ion currents for a reference spirolide, 13-desmethyl-C, was studied. In all quantitative experiments, excellent linearities in the concentration range between 0.01 and 1.75 microg/mL were obtained, with R2 values of 0.99 or higher. The average precision of the quantitative MALDI measurements was 7.4+/-2.4% RSD. No systematic errors were apparent with this method as shown by a direct comparison to an electrospray LC/MS/MS method. Most importantly, the MALDI technique was very fast; each sample spot was analyzed in less than 5 s as compared to several minutes with the electrospray assay. To demonstrate the potential of the MALDI triple quadrupole method, its application to quantitative analysis in several different phytoplankton samples was investigated, including crude extracts and samples from mass-triggered fractionation experiments. 13-Desmethyl spirolide C was successfully quantified in these complex samples at concentration levels from 0.05 to 90.4 microg/mL (prior to dilution to have samples fall within the dynamic range of the method) without extensive sample preparation steps. The versatility of the MALDI triple quadrupole method was also exhibited for the identification of unknown spirolide analogues. Through the use of dedicated linked scan functions such as precursor ion and neutral loss scans, several spirolide compounds were tentatively identified directly from the crude extract, without the usual time-consuming chromatographic preseparation steps. Moreover, high-quality CID spectra were obtained for low-abundant spirolides present in the phytoplankton samples.     

Biodiesel production from mixtures of canola oil and used cooking oil

Used cooking oil (UCO) was mixed with canola oil at various ratios in order to make use of used cooking oil for production of biodiesel and also lower the cost of biodiesel production. Methyl and ethyl esters were prepared by means of KOH-catalyzed transesterification from the mixtures of both the oils. Water content, acid value and viscosity of most esters met ASTM standard except for ethyl esters prepared from used cooking oil. Canola oil content of at least 60% in the used cooking oil/canola oil feedstock is required in order to produce ethyl ester satisfying ASTM specifications. Although ethanolysis was proved to be more challenging, ethyl esters showed reduced crystallization temperature (−45.0 to −54.4 °C) as compared to methyl esters (−35.3 to −43.0 °C). A somewhat better low-temperature property of ester was observed at higher used cooking oil to canola oil ratio in spite of similar fatty acid compositions of both oils.     

Pilocarpine‐loaded poly(DL‐lactic‐co‐glycolic acid) nanoparticles as potential candidates for controlled drug delivery with enhanced ocular pharmacological response

The poor corneal residence time of pilocarpine, an alkaloid extracted from the leaves of the Jaborandi plant, limits its ocular application. The aim of this study was to develop, characterize, and evaluate the potential of pilocarpine entrapped by poly(DL ‐lactic‐co‐glycolic acid) (PLGA) nanoparticle carriers for ocular drug delivery. Pilocarpine‐loaded nanoparticles were prepared with a double‐emulsion (water in oil in water) method and characterized with transmission electron microscopy and X‐ray diffraction analysis. The nanoparticles exhibited an average size of 82.7 nm with an encapsulation efficiency of 57%. Stability studies showed the absence of agglomeration and constancy in the amount of drug entrapped; this indicated the solidity of these particles for long‐term use. The in vitro release studies conducted in simulated tear fluid showed the sustained release of pilocarpine. In vivo evaluation of the nanoparticles was done in a rabbit model with a miosis assay and compared to an equal dose of commercially available eye drops of pilocarpine (Pilocar drops). The in vivo miosis studies showed that the duration of miotic response increased by 40% for the nanoparticles and produced an almost 68% increase in total miotic response when compared to the eye drops. In conclusion, this study clearly demonstrated the potential of pilocarpine‐loaded PLGA nanoparticles for multiplying the therapeutic effect of ophthalmic drug delivery with enhanced bioavailability and pharmacological response. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Efficiency enhancement in DSSC using metal nanoparticles: A size dependent study

The photoelectrode of Eosin-Y sensitised DSSC was modified by incorporating Au-nanoparticles to enhance the power conversion efficiency via scattering from surface plasmon polaritons. Size dependence of Au nanoparticle on conversion efficiency was performed in DSSC for the first time by varying the particle size from 20 to 94 nm. It was found that, the conversion efficiency is highly dependent on the size of the Au nanoparticles. For larger particles (>50 nm), the efficiency was found to be increased due to constructive interference between the transmitted and scattered waves from the Au nanoparticle while for smaller particles, the efficiency decreases due to destructive interference. Also a reduction in the V_oc was observed in general, due to the negative shifting of the TiO₂ Fermi level on the adsorption of Au nanoparticle. This shift was negligible for larger particles. When 94 nm size particles were employed the conversion efficiency was doubled from 0.74% to 1.52%. This study points towards the application of the scattering effect of metal nanoparticle to enhance the conversion efficiency in DSSCs.     

Comparison of MALDI to ESI on a triple quadrupole platform for pharmacokinetic analyses

This present work describes the systematic experimental comparison of electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI) for pharmacokinetic (PK) analysis of two drug candidates from rat plasma using single reaction monitoring (SRM) on a triple quadrupole mass spectrometer. The electrospray assay is an established method using a fast liquid chromatography (LC) separation of the sample extracts prior to mass spectrometry analysis. The novel MALDI assays measured the concentration levels of the drug candidates directly from the spotted sample extracts. Importantly, for both LC-ESI and MALDI the same solid-phase sample extraction protocol, internal standards, triple quadrupole mass analyzer platform, and SRM conditions were used, thus effectively standardizing all experimental parameters of the two assays. Initially, analytical figures of merit such as linearity, limit of quantitation, precision, and accuracy were determined from the calibration curves, indicating very similar performance for both LC-ESI and MALDI. Moreover, the LC-ESI rat plasma concentration time profiles of the drug candidates after orally dosing the animals were accurately reproduced by the MALDI assay, giving virtually identical PK results. The direct MALDI assay, however, was able to generate the data at least 50 x faster than the LC-ESI assay. It is shown in this study that analyzing the entire PK curve for one animal took less than 2 min using MALDI (with five replicate analyses per sample), whereas the corresponding LC-ESI assay required 80 min, however, allowing only two replicate measurements in that time frame.     

Size dependent electron transfer from CdTe quantum dots linked to TiO2 thin films in quantum dot sensitized solar cells

In this present study, we demonstrate the size dependent charge transfer from CdTe quantum dots (QDs) into TiO₂ substrate and relate this charge transfer to the actual behavior of a CdTe sensitized solar cell. CdTe QDs was synthesized using mercaptopropionic acid as the capping agent. The conduction band offset for TiO₂ and CdTe QDs indicates thermodynamically favorable band edge positions for smaller QDs for the electron-transfer at the QD–TiO₂ interface. Time-resolved emission studies were carried out for CdTe QD on glass and CdTe QD on TiO₂ substrates. Results on the quenching of QD luminescence, which relates to the transfer kinetics of electrons from the QD to the TiO₂ film, showed that at the smaller QD sizes the transfer kinetics are much more rapid than at the larger sizes. I–V characteristics of quantum dot sensitized solar cells (QDSSC) with different sized QDs were also investigated indicating higher current densities at smaller QD sizes consistent with the charge transfer results. The maximum injection rate constant and photocurrent were obtained for 2.5 nm CdTe QDs. We have been able to construct a solar cell with reasonable characteristics (V_oc = 0.8 V, J_sc = 1 mA cm⁻², FF = 60%, η = 0.5%).     

Structural,Dielectric,and Magnetic Studies on Electrospun Magnesium Ferrite-Polyvinylidene Fluoride Core–Shell Composite Fibers

The sub-micron(of the order of 150 nm) thick core–shell composite fibers of magnesium ferrite-polyvinylidene fluoride are prepared by electrospinning.The loading of magnesium ferrite is varied from 1 to 10 wt%.The study results by X-ray diffraction,scanning electron microscope,and infra-red spectroscopy indicate the formation of core–shell structure and an enhancement in the amount of b-phase compared to a-phase in the polyvinylidene fluoride.The particle size of the magnesium ferrite in the fiber is evaluated to be 30 nm.The low frequency dielectric studies indicate that the addition of the magnesium ferrite increases the polarization resulting in the increase in the dielectric constant but decreases the dielectric loss.The magnetization measurements indicate an increased value of coercivity compared to bulk due to the nano-size of the magnesium ferrite.The microwave absorption at the ferromagnetic resonance increases with the increase in the concentration of magnesium ferrite.The resonance field is found to vary with the loading of MFO.