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Background: Wheat bran is rich in dietary fiber (DF), particularly insoluble dietary fiber (IDF). Although the benefits for human health following the consumption of these DFs have been documented, the lower water retention capacity (WRC) and other properties still limit the applications of DF. Therefore, the current research investigated the impact of acetylation on the changes in the corresponding physicochemical and functional properties of DF., Results: The current results indicated the acetylated group restricted the alignment of the molecular chains, which led to an increased amorphous phase in the fiber structure, followed by an enhanced thermal sensitivity and a reduced crystallinity as evidenced by X-ray diffraction (XRD). Moreover, the acetylation of the IDFs enhanced the cholesterol absorption capacity, but the corresponding antioxidant capacity and cation exchange capacity were reduced, which might be due to the partial loss of the phenolic compounds onto the polysaccharides during the modification. Interestingly, a lower degree of substitution (DS) of the IDF achieved from water-acetic anhydride modification led to a higher WRC and water swelling capacity (WSC). In contrast, a higher DS from acetic anhydride modification demonstrated a greatly improved in vitro hypoglycemic performance of the IDF, including α-amylase inhibitory activity and glucose dialysis retardation index (GDRI), compared to the other samples., Conclusion: This study highlights a new approach to modify the functionality of IDFs via acetylation and the design of a novel IDF with hypoglycemic activity. © 2023 Society of Chemical Industry., (© 2023 Society of Chemical Industry.)

Grapefruit peel polysaccharide has antioxidant, antitumor, hypoglycemic and other biological activities, and chemical modification can further improve the properties of the polysaccharide. Acetylation modification of polysaccharides has the advantages of simple operation, low cost and little pollution, and is widely used at present. Different degrees of acetylation modification have different effects on the properties of polysaccharides, so it is necessary to optimize the preparation technology of acetylated grapefruit peel polysaccharides. In this article, acetylated grapefruit peel polysaccharide was prepared by acetic anhydride method. With the degree of acetyl substitution as the evaluation index, combined with the analysis of sugar content and protein content in the polysaccharide before and after modification, the effects of three feeding ratios of 1:0.6, 1 : 1.2 and 1 : 1.8 (polysaccharide: acetic anhydride, mass/volume) on acetylation modification were explored through single factor experiments. The results showed that the optimum ratio of material to liquid for acetylation modification of grapefruit peel polysaccharide was 1:0.6. Under these conditions, the degree of substitution of acetylated grapefruit peel polysaccharide was 0.323, the sugar content was 59.50 % and the protein content was 1.038 %. The results provide some reference for the study of acetylated grapefruit peel polysaccharide., (© 2023 Wiley-VHCA AG, Zurich, Switzerland.)

Protein acetylation is a significant post-translational modification, and hyperacetylation results in amyloid aggregation, which is closely related to neurodegenerative diseases (Alzheimer's disease, Huntington's disease, and so on). Therefore, it is significant to inhibit the hyperacetylation of proteins and their induced aggregation. In the present study, we aimed to explore the anti-acetylation and anti-amyloid properties of five small molecules (gallic acid, menadione, resveratrol, apigenin, and quercetin) in the process of acetic anhydride-induced protein hyperacetylation and its aggregation. Optical detection methods, such as SDS-PAGE, inverted fluorescence microscopy, and endogenous fluorescence spectroscopy, were used to investigate the effects of small molecules on protein acetylation, aggregation, and structure. In addition, fluorescence quenching and molecular docking techniques were used to explore the relationship between small molecules and acetylation. The results showed that gallic acid (200 μM), menadione (100 μM), quercetin (40 μM), resveratrol (5 μM), and apigenin (20 μM) (unmodified rates were 61.12 %, 67.76 %, 65.11 %, 62.66 %, and 67.81 %, respectively) had strong inhibitory effects on acetylation, and there was no significant difference (P < 0.05). In addition, gallic acid (200 μM), menadione (100 μM), and resveratrol (5 μM) (inhibition rates of 29.89 %, 26.53 %, and 26.09 %, respectively) had more substantial inhibitory effects on protein aggregation, indicating that the five small molecules could inhibit acetic anhydride-induced hyperacetylation and protein aggregation. The underlying mechanism might be that it could inhibit hyperacetylation and resist amyloid aggregation by interacting with proteins to occupy acetylation sites. Collectively, our findings showed that gallic acid, menadione, and resveratrol could potentially prevent and treat neurodegenerative diseases, such as Alzheimer's disease, by inhibiting acetylation and acetylation-induced aggregation., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Chemical modifications of Scots pine (Pinus slyvestris) wood flour were performed with vinyl acetate (VA) and acetic anhydride (AA) in the presence of potassium carbonate as a catalyst. Scots pine wood flour samples were successfully acetylated with VA (19 wt% gain) and AA (24 wt% gain). The effect of chemical modification of the Scots pine wood flour with AA and VA on the mechanical properties of wood high-density polyethylene composites (WPC) were determined. It was observed that acetylation of wood flour allowed a significant increase in both the mechanical properties and the thermal stability of the WPCs. It was concluded that acetylation of lignocellulosic fibers improves thermal stability, dispersion in the polymer matrix, and compatibility with the polymer matrix.

The aim of this work was to study the influence of the acetylation process of kraft lignin on developing dispersions potentially applicable as new bio-based semisolid lubricants. Lignin was functionalized with acetic anhydride and pyridine as a catalyst by modifying different reaction variables (temperature, ratio of pyridine/acetic anhydride and time). Acetylated lignin was analyzed using FTIR, 1 H and 13 C NMR techniques, TGA, DSC and SEM to evaluate the chemical, morphological and thermal changes induced by the acetylation process. The influence of the acetylation process on the rheological and tribological properties of dispersions was related to the development of different microstructures, which depend on chemical and morphological properties of acetylated lignin. In this sense, two different rheological behaviours (gel-like or fluid-like) were found to depend on the reaction time. From the experimental results obtained, it can be concluded that the acetylation process is a key issue to modulate rheological and morphological properties of dispersions, resulting in an effective method to improve the compatibility of lignin and castor oil. Acetylated lignin with medium degrees of substitution with adequate morphological properties can be potentially used as an effective thickening agent to develop semisolid lubricants., Competing Interests: Declaration of competing interest There are no interests to declare: ‘Declarations of interest: none’., (Copyright © 2022. Published by Elsevier B.V.)

Presented is the analysis of four cannabinoid-based products. These products were part of a case involving visual and auditory hallucinations that precipitated the commission of a felony and subsequent arrest. The products were labeled to contain ∆8-tetrahydrocannabinol (∆8-THC) or THC acetate (THC-O-A). Primary reference materials were not available for ∆8-THC-O-A, ∆10-THC-O-A, cannabidiol di-acetate (CBD-di-O-A) or respective deuterated internal standards. THC-O-A and CBD-di-O-A standards were prepared by derivatizing ∆8-THC, ∆9-THC, ∆10-THC, CBD, ∆9-THC-d3 and CBD-d3 using acetic anhydride. The cannabinoid-based products were determined to contain ∆8-THC, ∆8-THC-O-A, ∆9-THC-O-A and CBD-di-O-A and/or other phytocannabinoids using three different analytical techniques. Direct analysis in real-time-time-of-flight mass spectrometry was used for identifying exact masses. A gas chromatograph-mass spectrometer was used for the identification of compounds and to quantitate THC-O-As in the products. A liquid chromatograph-tandem mass spectrometer was used to identify and quantitate phytocannabinoids and CBD-di-O-A in the products. To the authors' knowledge, this is the first case report involving the identification of THC-O-As and CBD-di-O-A in commercially available products. Minimal clinical/pharmacological data is available for these emerging synthetic cannabinoids/novel psychoactive substances., (© The Author(s) 2022. Published by Oxford University Press. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.)

A novel GC-MS/MS analytical method was established for the qualitative and quantitative determination of tilmicosin in poultry (Jinghai yellow chicken, Gaoyou duck and Yangzhou goose) eggs. The method was based on LLE and SPE for sample extraction and purification. Pyridine and acetic anhydride were used for the derivatization reaction. When tilmicosin was added to blank poultry egg samples at the LOQ and 75 μg/kg, 150 μg/kg, and 300 μg/kg, the recoveries ranged from 72.80% to 88.75%, the intraday and interday RSDs ranged from 2.31% to 4.56% and 3.29%-5.61%, respectively, and the LODs and LOQs ranged from 3.8 to 5.6 μg/kg and 8.4-10.5 μg/kg, respectively. These results confirmed that the parameters of this novel method meet the requirements of the FAO & WHO (2014) for veterinary drug residue testing. Poultry egg samples purchased from the local market were analysed according to the established method and only one egg sample was found to contain 18.9 μg/kg of tilmicosin., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Chemical modifications of Scots pine (Pinus sylvestris) wood flour were performed with vinyl acetate (VA) and acetic anhydride (AA) in the presence of potassium carbonate as a catalyst. Scots pine wood flour samples were successfully acetylated with VA (19 wt% gain) and AA (24 wt% gain). The effect of chemical modification of the Scots pine wood flour with AA and VA on the mechanical properties of wood high-density polyethylene composites (WPC) was determined. It was observed that acetylation of wood flour allowed a significant increase in both the mechanical properties and the thermal stability of the WPCs. It was concluded that acetylation of lignocellulosic fibers improves thermal stability, dispersion in the polymer matrix, and compatibility with the polymer matrix. [ABSTRACT FROM AUTHOR]

Reaction of glycine-based dithiocarbamates with nitroalkenes in the presence of acetic anhydride was utilized for the synthesis of fully substituted 2-(alkylsulfanyl)-4-(nitroalkyl)-5-acyloxy-1,3-thiazoles. The reaction proceeds via the in situ formation of thiazol-5(4 H )-one from glycine-based dithiocarbamates, followed by the Michael addition of this intermediate to nitroalkenes, aromatization, and esterification reaction cascade. This new one-pot three-component reaction afforded a diverse library of fully substituted thiazoles in high to excellent yields under solvent-free conditions.

An efficient method for the acylation and formylation of alcohols and phenols by using an acylating/formylating agent (acetic anhydride and formic acid) in the presence of a catalytic amount of N,N'-dibromo-N,N'-1,2-ethanediylbis(benzene sulfonamide) under mild and solvent-free conditions at room temperature in good to excellent yields is described. The use of protic acids and metal Lewis acids is avoided. [ABSTRACT FROM AUTHOR]

Abstract: An efficient method for the acylation of alcohols by using acetic anhydride and a catalytic amounts of 1,3-dibromo-5,5-dimethylhydantoin and/or trichloroisocyanuric acid under mild and heterogeneous conditions at room temperature described in good to excellent yields. [Copyright &y& Elsevier]

Abstract: N,N-Dibromo-4-methylbenzenesulphonimide efficiently catalyzes acylation of structurally diverse alcohols by the action of acetic anhydride in chloroform at room temperature. [Copyright &y& Elsevier]

New acetyl derivatives of uracil, 6-methyluracil, and thymine were obtained in the course of an unconventional synthesis in methylene chloride. It was shown that products with the acetyloxymethyl fragment are formed according to a mechanism different from that for products with the acetyloxyethyl group. In particular, for uracil it was proven that the reaction with Ac 2 O, TEA, and CH 2 Cl 2 leads to 1-acetyloxymethyluracil, where the N 1 substituent is composed of the -CH 2 - fragment that originated from CH 2 Cl 2 and the 1-acetyloxy moiety from Ac 2 O. The reaction of uracil with Ac 2 O, TEA, CH 2 Cl 2 , and DMAP leads to an acetyloxyethyl derivative in which the -CH 2 -CH 2 - fragment originates from TEA and the 1-acetyloxy moiety from Ac 2 O. A possible mechanism for the formation of new compounds was suggested and supported by the density functional theory/B3LYP quantum mechanical calculations. New compounds (39 in total, including seven deuterated) were fully characterized by nuclear magnetic resonance and high-resolution mass spectrometry techniques.

The purpose of the present study was to determine the effects of acetylation with different doses of acetic anhydride on the chemical composition and chosen functional properties of commercial pumpkin protein concentrate (PPC). The total protein content decreased as compared to unmodified samples. Electrophoretic analysis revealed that in the acetylated pumpkin protein, the content of the heaviest protein (35 kDa) decreased in line with increasing concentrations of modifying reagent. Acetylation of PPC caused a significant increase in water-binding and oil-absorption capacity and for emulsifying properties even at the dose of 0.4 mL/g. Additionally, an increase in foaming capacity was demonstrated for preparations obtained with 2.0 mL/g of acetic anhydride, whereas acetylation with 0.4 and 1.0 mL/g caused a decrease in protein solubility as compared to native PPC.

In this work, an emerging and efficient strategy for the preparation of lignin samples with different acetylation degree by choline chloride/acetic anhydride (ChCl/Aa) treatment of pine kraft lignin (PKL) is reported, and the effects of efficient pre-acetylation of hydroxyl functional groups on subsequent lignin pyrolysis are also systematically investigated. The results show that the ChCl/Aa displays a high acetylation efficiency towards the aliphatic hydroxyl (~99.1%) and phenolic hydroxyl (~94.0%) of PKL, which enhances the hydrogen to carbon effective ratio of PKL. Noticeably, the ChCl/Aa has a slight effect on β-O-4 of PKL, and the acetylation of hydroxyl is beneficial for the improvement of the maximum degradation rate of PKL. In addition, the acetylation of hydroxyl is also significantly contributed to the increment of the pyrolysis bio-oil yield. Importantly, the relative content of the H-phenols obtained from acetylated lignins pyrolysis shows a positive correlation with the acetylation degree of hydroxyl., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Phenethyl ester is an important contributors to food, drinks, cosmetics and perfumery. Phenethyl acetate was synthesized enzymatically from phenethyl alcohol with acyl donors catalyzed by Novozym 435 from Candida antarctica lipase B. Through acyl donor screening, acetic anhydride and vinyl acetate were found to be the optimal acyl donors for the reaction. The effects of the molar ratio, temperature and solvents were investigated. The maximum conversion of phenethyl acetate were 99.12%, and 98.44%, using acetic anhydride and vinyl acetate as the acyl donors, respectively. After 20 reuses, the respective conversion of phenethyl acetate were 97.62% and 96.52%. This study may contribute to environment-friendly synthesis of phenethyl ester based on optimal conditions, and enzyme reusability for high conversion of phenethyl acetate., (Copyright © 2017 Elsevier Inc. All rights reserved.)

A method based on the combination of hollow fiber liquid-liquid-liquid microextraction and solid-phase microextraction (SPME) followed by gas chromatography-electron capture detection was developed for the determination of chlorophenols in water and wastewater samples. Silica microstructures fabricated on the surface of a stainless steel wire were coated by an organic solvent and used as a SPME fiber. The analytes were extracted through a hollow fiber membrane containing n-decane from sample solution to an alkaline aqueous acceptor phase. They were then extracted and in situ derivatized on the SPME fiber using acetic anhydride. Experimental parameters such as the type of extraction solvent, acceptor phase NaOH concentration, donor phase HCl concentration, the amount of derivatizing reagent, salt concentration, stirring rate and extraction time were investigated and optimized. The precision of the method for the analytes at 0.02-30μgL(-1) concentration level ranged from 7.1 to 10.2% (as intra-day relative standard deviation) and 6.4 to 9.8% (as inter-day relative standard deviation). The linear dynamic ranges were in the interval of 5-500μgL(-1), 0.05-5μgL(-1), 0.02-1μgL(-1) and 0.001-0.5μgL(-1) for 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol, respectively. The enrichment factors were between 432 and 785. The limits of detection were in the range of 0.0004-1.2μgL(-1). Tap water, well water and wastewater samples were also analyzed to evaluate the method capability for real sample analysis., (Copyright © 2015 Elsevier B.V. All rights reserved.)

During automated solid-phase peptide synthesis, failure sequences were capped with acetic anhydride. After synthesis, a polymerizable methacrylamide tag was attached to the full-length sequences. Peptide purification was then achieved by polymerizing the full-length sequences, washing away impurities, and cleaving the peptide product from the polymer.

We report a facile approach to synthesizing 3-aminopropyltrimethoxysilane (APTS)-coated magnetic iron oxide (Fe(3)O(4)@APTS) nanoparticles (NPs) with tunable surface functional groups for potential biomedical applications. The Fe(3)O(4) NPs with a mean diameter of 6.5 nm were synthesized by a hydrothermal route in the presence of APTS. The formed amine-surfaced Fe(3)O(4)@APTS NPs were further chemically modified with acetic anhydride and succinic anhydride to generate neutral (Fe(3)O(4)@APTS⋅Ac) and negatively charged (Fe(3)O(4)@APTS⋅SAH) NPs. These differently functionalized NPs were extensively characterized by x-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, thermogravimetry analysis, zeta potential measurements, and T(2) relaxometry. The cytotoxicity of the particles was evaluated by in vitro 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide colorimetric viability assay of cells along with microscopic observation of cell morphology. The hemocompatibility of the particles was assessed by in vitro hemolysis assay. We show that the hydrothermal approach enables an efficient modification of APTS onto the Fe(3)O(4) NP surfaces and the formed NPs with different surface charge polarities are water-dispersible and colloidally stable. The acetylated Fe(3)O(4)@APTS⋅Ac NPs displayed good biocompatibility and hemocompatibility in the concentration range of 0-100 µg ml(-1), while the pristine Fe(3)O(4)@APTS and Fe(3)O(4)@APTS⋅SAH particles started to display slight cytotoxicity at a concentration of 10 µg ml(-1). The findings from this study suggest that the Fe(3)O(4)@APTS NPs synthesized by the one-pot hydrothermal route can be surface modified for various potential biomedical applications.

Direct benzoylation of the two hydroxyl groups on chitosan was achieved using a phosphoryl mixed anhydride system, derived from trifluoroacetic anhydride (TFAA), benzoic acids (BAs), and phosphoric acid (PA). The reaction is operated as a one pot process under mild conditions that does not require neither an inert atmosphere nor dry solvents. The structures of the synthesized compounds were confirmed by NMR and IR spectroscopy. Solubility tests on the products revealed that they were soluble in organic solvents such as N,N-dimethylformamide (DMF), dimethylsulfoxide (DMSO), and acetone. In the meantime, a morphological study by scanning electron microscopy (SEM) evidently indicated that the chitosan benzoates underwent significant structural changes after the benzoylation.

The use of perfluorinated anhydrides coupled with perfluoroalcohols for the derivatization of cannabinoids has been well documented. Derivatization is used in the detection of cannabinoids using gas chromatography-mass spectrometry (GC-MS) with both electron impact ionization (EI) and negative chemical ionization (NCI). During method development for the analysis of cannabinoids in biological samples using GC-MS in EI and NCI mode, it was observed that when Δ(9)-tetrahydrocannabinol (THC) and cannabidiol (CBD) were derivatized with trifluoroacetic anhydride (TFAA), the resultant derivatives produced the same retention times and mass spectra. This was not observed with the trimethylsilyl (TMS) derivatives of THC and CBD. This complication is due to the conversion of CBD to THC under acidic conditions. The work here highlights the unsuitability of the derivatizing reagent TFAA for the detection of THC and CBD. For the analysis of case samples, even if only THC is of interest, the presence of CBD cannot be excluded, and other derivatization techniques should be used.

We report a facile protocol to obtain 22-substituted furostans and pseudosapogenins in high yields from (25R)- and (25S)-sapogenins. This method involves the treatment of the sapogenin with acetic-trifluoroacetic mixed anhydride and BF(3)·OEt(2) at room temperature, followed by the addition of a nucleophile (H(2)O, MeOH or KSeCN). In the case of 22-hydroxyfurostans, they can be transformed to pseudosapogenins by treatment with p-toluensulfonic acid., (Copyright © 2011 Elsevier Inc. All rights reserved.)

A simple, rapid and sensitive method termed dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography-mass spectrometry (GC/MS) was developed for the determination of tricyclic antidepressants (TCAs) in human urine sample. An appropriate mixture of methanol (disperser solvent), carbon tetrachloride (extraction solvent), and acetic anhydride (derivatization reagent) was injected rapidly into human urine sample. After extraction, the sedimented phase was analyzed by GC/MS. The calibration curves obtained with human urine were linear with a correlation coefficient of over 0.99 in the range of 2.0/5.0-100 ng mL(-1). Under the optimum conditions (carbon tetrachloride: 10 μL, methanol: 150 μL), the detection limits and the quantification limits of the tricyclic antidepressants were 0.5-2.0 ng mL(-1) and 2.0-5.0 ng mL(-1), respectively. The average recoveries of TCAs were 88.2-104.3%. Moreover, the inter- and intra-day precision and accuracy was acceptable at all concentrations. The results showed that DLLME is applicable to the determination of trace amounts of TCAs in human urine sample., (Copyright © 2011 Elsevier B.V. All rights reserved.)

Avermectines are antiparasitic agents widely used as veterinary drugs for food producing animals. The European Community, due to their side effects, limited the use of these molecules establishing maximum residue limits (MRLs) in some foods. A validated qualitative and quantitative high performance liquid chromatography method with fluorescence detection (HPLC-FL) is presented for the simultaneous determination of ivermectin (IVM), abemectin (ABA), moxidectin (MOX), eprinomectin (EPR), doramectin (DOR) and emamectin (EMA) in foodstuffs (muscle, eggs and milk). Samples were extracted with acetonitrile, purified with liquid-liquid extraction (LLE), and analysed by HLPC-FL previous derivatization with trifluoroacetic anhydride (TFAA) in presence of 1-methyl-imidazole (MI) and acetic acid. To date, the presented method is the first validated for the matrix eggs, and in accordance with the requirements set by Commission Decision 2002/657/EC. Recoveries of the methods, calculated spiking the samples in the range 5.0-100.0 μg kg(-1), were 64-83% for muscle, 65-89% for milk and 63-84% for eggs. The precision (CV) ranged between 9.2 and 17.1% for muscle, 9.9 and 16.6% for milk and from 9.4 to 17.4% for eggs. Linearity for the six analytes was calculated from 5.0 to 200.0 μg kg(-1). The main advantages of the presented method are its rapidity, the specificity, the good precision and recovery that make it very suitable to the detection and determination of avermectines., (Copyright © 2011 Elsevier B.V. All rights reserved.)

A combination of dimethyl sulfoxide (DMSO) and trifluoroacetic anhydride (TFAA) mediates functionalization at the 2α-position of indole derivatives. Carbon and heteroatom nucleophiles were directly introduced via a one-pot procedure in excellent yields., (This journal is © The Royal Society of Chemistry 2011)

A smooth and efficient oxidation of isonitriles to isocyanates by sulfoxides is catalyzed by trifluoroacetic anhydride. With use of DMSO as the oxidant and 5 mol·% TFAA (dichloromethane, -60 to 0 °C), the process is complete in a few minutes, forming dimethyl sulfide as the only byproduct. The newly formed isocyanates may be used directly or isolated in high purity by solvent evaporation.

Acylation of chitin with butyric acid was performed in the presence of trifluoroacetic anhydride/phosphoric acid mediated system. The products were characterized by (1)H NMR and FT-IR spectroscopy and their solubility was tested in different organic solvents. Inclusion of butyric acid moieties into the parent molecule was confirmed from the (1)H NMR and FT-IR spectra. FT-IR analysis revealed that the degree of acid substitution (DS) of the products was in a range of 1.9-2.38, which increased with increasing the amounts of butyric acid added to the reaction system. Degree of N-deacetylation (DD) of the products, as determined by (1)H NMR was between 54.2% and 65.6%. The products with DS >2.0 were soluble in dimethyl sulfoxide, N,N-dimethylformamide, tetrahydrofuran, methanol, acetone, chloroform, and acetic acid., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

Endogenous nitro-fatty acids, acting as partial agonist of PPARγ, are able to lower the insulin and glucose levels without the side effects associated with common antidiabetic drugs. (E)-12-Nitrooctadec-12-enoic acid, a potent activator of this peroxisome receptor, was synthesized in a very efficient sequence via a Henry-retro-Claisen ring fragmentation, followed by a novel enzymatic cleavage of methyl esters. The latter method was then applied in the last step of the synthesis of a few labile natural products, such as prostaglandins, isoprostanes, and phytoprostanes.

A dispersive liquid-liquid microextraction (DLLME) method has been optimised for simultaneously extracting 2,4,6-trichloranisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA), pentachloroanisole (PCA), 2,4,6-trichlorophenol (TCP), 2,3,4,6-tetrachlorophenol (TeCP), 2,4,6-tribromophenol (TBP) and pentachlorophenol (PCP) from wine. The haloanisoles and halophenols were automatically determined using a gas chromatography-electron-capture detection (GC-ECD) system. Derivatisation of halophenols was performed at the same time as DLLME. Firstly, disperser and extraction solvents, salt addition and temperature conditions were selected. Then, the volume of disperser solvent, extraction solvent and derivatisation agent, and the percentage of base were optimised by means of a central composite design combined with desirability functions. The optimal extraction-derivatisation conditions found were 1.3 mL of acetone, 150 μL of carbon tetrachloride, 75 μL of acetic anhydride and a percentage of base of 0.7%; with no salt addition and at room temperature. Under these conditions, the proposed method showed satisfactory linearity (with correlation coefficients over 0.994), repeatability (below 9.7%) and reproducibility (below 9.9%). Moreover, detection limits were lower than the olfactory threshold of the compounds. The developed method was successfully applied to the analysis of red wine samples. To our knowledge, this is the first time that DLLME has been applied to determine cork taint responsible compounds in wine., (Copyright © 2010 Elsevier B.V. All rights reserved.)

Chickpea protein concentrate was acetylated with acetic anhydride at 5 levels. Acetylated chickpea protein (ACP) dispersions at 3 levels (6%, 45%, and 49%) were chosen for this flow property study. Effects of protein concentration, temperature, concentrations of salt addition and particularly, degree of acetylation on these properties were examined. Compared with native chickpea proteins, the ACP dispersions exhibited a strong shear thinning behavior. Within measured temperature range (15 to 55 degrees C), the apparent viscosities of native chickpea protein dispersions were temperature independent; those of ACP dispersions were thermally affected. The flow index (n), consistency coefficient (m), apparent yield stress, and apparent viscosities of ACP dispersions increased progressively up to 45% acetylation but decreased at 49% acetylation level. Conformational studies by gel filtration suggested that chickpea proteins were associated or polymerized at up to 45% acetylation but the associated subunits gradually dissociated to smaller units at higher levels (49%) of acetylation.

Reaction screening of nucleophilic reaction partners for addition to N-diphenylphosphinylimines employing lanthanum(III) triflate as a catalyst and trifluoroacetic anhydride (TFAA) as an activator is reported. A number of tandem processes leading to novel chemotypes including aza-Prins/intramolecular Friedel-Crafts annulations have been identified, and both reaction scope and mechanism further investigated.

Studies on the aggregation of mutant proteins have provided new insights into the genetics of amyloid diseases and the role of the net charge of the protein on the rate, extent, and type of aggregate formation. In the present work, hen egg white lysozyme (HEWL) was employed as the model protein. Acetylation and (separately) citraconylation were employed to neutralize the charge on lysine residues. Acetylation of the lysine residues promoted amyloid formation, resulting in more pronounced fibrils and a dramatic decline in the nucleation time. In contrast, citraconylation produced the opposite effect. In both cases, native secondary and tertiary structures appeared to be retained. Studies on the effect of pH on aggregation suggested greater possibilities for amorphous aggregate formation rather than fibrillation at pH values closer to neutrality, in which the protein is known to take up a conformation more similar to its native form. This is in accord with reports in the literature suggesting that formation of amorphous aggregates is more favored under relatively more native conditions. pH 5 provided a critical environment in which a mixture of amorphous and fibrillar structures were observed. Use of Tango and Aggrescan software which describe aggregation tendencies of different parts of a protein structure suggested critical importance of some of the lysine residues in the aggregation process. Results are discussed in terms of the importance of the net charge in control of protein-protein interactions leading to aggregate formation and possible specific roles of lysine residues 96 and 97., (Copyright 2009 Elsevier B.V. All rights reserved.)

Mephentermine and phentermine, substances prohibited in sports by the World Anti-Doping Agency, were found for the first time in urine specimens following the administration of a therapeutic medication, oxethazaine. In a recent sporting event, a urine specimen donor who tested positive for mephentermine and phentermine claimed consumption of Mucaine((R)) for treating stomach pain was the reason for testing positive. Five volunteers were administrated oxethazaine (a topical anesthetic found in the multi-ingredient medication Mucaine and its generic equivalent, Stoin, both of which are available in Taiwan), mephentermine, and phentermine. Excretion profiles of mephentermine and phentermine following the administration of these drugs were found to be similar. However, the mephentermine/phentermine ratios found in urine specimens collected at different time points following the administration of oxethazine and mephentermine were found to be characteristically different.