The rheological and thickening properties of cationic xanthan gum

In the present study, cationic xanthan gum (CXG) was synthesized to enhance the rheological property of xanthan gum (XG) by attaching quaternary amine groups to the backbone of XG. The efficacy of the substitution was confirmed by FT-IR spectra and ¹³C NMR. The surface morphology was changed considerably as demonstrated by SEM. The examined rheological properties of XG and CXG include steady-state and dynamic rheological properties. The results show that quaternary amine groups are successfully grafted onto the XG molecule. Apparent viscosity, storage modulus, and loss modulus of CXG solutions are greater than those of XG solutions under the same conditions. It is moreover found that apparent viscosity and viscoelasticity increase with the degree of substitution. The data indicate that the modified XG has much better heat resistance.     

Xanthan Gum Production by <Emphasis Type="Italic">Xanthomonas campestris pv. campestris</Emphasis> IBSBF 1866 and 1867 from Lignocellulosic Agroindustrial Wastes

This study aimed to evaluate the properties of xanthan gum produced by Xanthomonas campestris pv. campestris 1866 and 1867 from lignocellulosic agroindustrial wastes. XG was produced using an orbital shaker in a culture medium containing coconut shell (CS), cocoa husks (CH), or sucrose (S) minimally supplemented with urea and potassium. The XG production results varied between the CS, CH, and S means, and it was higher with the CH in strains 1866 (4.48 g L^?1) and 1867 (3.89 g L^?1). However, there was more apparent viscosity in the S gum (181.88 mPas) and the CS gum (112.06 mPas) for both 1866 and 1867, respectively. The ability of XG_CS and XG_CH to emulsify different vegetable oils was similar to the ability of XG_S. All gums exhibited good thermal stability and marked groups in the elucidation of compounds and particles with rough surfaces.     

A Study of the Effects of Aeration and Agitation on the Properties and Production of Xanthan Gum from Crude Glycerin Derived from Biodiesel Using the Response Surface Methodology

The effects of aeration and agitation on the properties and production of xanthan gum from crude glycerin biodiesel (CGB) by Xanthomonas campestris mangiferaeindicae 2103 were investigated and optimized using a response surface methodology. The xanthan gum was produced from CGB in a bioreactor at 28 °C for 120 h. Optimization procedures indicated that 0.97 vvm at 497.76 rpm resulted in a xanthan gum production of 5.59 g L^?1 and 1.05 vvm at 484.75 rpm maximized the biomass to 3.26 g L^?1. Moreover, the combination of 1.05 vvm at 499.40 rpm maximized the viscosity of xanthan at 0.5 % (m/v), 25 °C, and 25 s^?1 (255.40 mPa s). The other responses did not generate predictive models. Low agitation contributed to the increase of xanthan gum production, biomass, viscosity, molecular mass, and the pyruvic acid concentration. Increases in the agitation contributed to the formation of xanthan gum with high mannose concentration. Decreases in the aeration contributed to the xanthan gum production and the formation of biopolymer with high mannose and glucose concentrations. Increases in aeration contributed to increased biomass, viscosity, and formation of xanthan gum with greater resistance to thermal degradation. Overall, aeration and agitation of CGB fermentation significantly influenced the production of xanthan gum and its properties.     

Studying the Interaction of Xanthan Gum and Pectin with Some Functional Carbohydrates on the Rheological Attributes of a Low-Fat Spread

Effects of xanthan gum (XG) (0.1 wt%) and pectin (PE) (0.5 wt%) alone and in combination with different concentrations (0.2 and 0.4 wt%) of locust bean gum (LBG), modified starch (MS), and Na-alginate (ALG) on some of the rheological characteristics of low-fat spreads, including flow behavior curves, rheological modeling, apparent viscosity, rheological modules (storage modulus (G′) and loss modulus (G″)), and delta degree (G″/G′) were studied. Results showed the power-law model was better than the Herschel–Bulkley model to describe the flow curve of dispersions. The k-value in the power-law model increased with increase in biopolymers concentration in solution. All samples exhibited shear-thinning flow behavior with a low yield stress. Dynamic oscillatory shear test showed that the spreads had a viscoelastic solid behavior with a gel-like structure. The G′ value was increased by increasing frequency from 0.03 to 15 Hz, while the G″ and G″/G′ values decreased. Also, MS in combination with XG and PE led to increase the G′ values of spreads in comparison with ALG and LBG. Moreover, microstructural and stability observations revealed that the spreads prepared with 0.1% XG-0.2% LBG significantly had the highest oiling out.     

Evaluation of the Counter Ions in Doped Porous Polyaniline Coatings on Stainless Steel Wires for Solid Phase Microextraction of Chlorophenolics in Water Combined with High-Performance Liquid Chromatography

Porous polyaniline coatings doped with different counter ions were electrodeposited on the surface of stainless steel wires using controlled potentiostatic coulometry. Prior to electropolymerization, the stainless steel wires were chemically etched to improve subsequent immobilization of the polyaniline coatings on the substrate and to increase the effective surface area. Porous polyaniline coatings doped with sulfate, nitrate, and perchlorate counter ions were employed for solid-phase microextraction (SPME) of 2-chlorophenol, 2,4-dichlorophenol, triclosan, and 2,4-dichlorophenoxyacetic acid coupled to high-performance liquid chromatography. The results demonstrated that the perchlorate doped polyaniline coating exhibited the highest extraction efficiency for 2-chlorophenol, 2,4-dichlorophenol, and triclosan at pH 5.0, indicating that the extraction capability was modified by introducing different counter ions into the coatings. As a result, the perchlorate doped polyaniline coated fiber was further used for the optimization of extraction condition s . The method provided linear dynamic ranges over 2 to 4 orders of magnitude. The limits of detection were 0.006 µg · L^?1, 0.005 µg · L^?1, and 0.040 µg · L^?1 for 2-chlorophenol, 2,4-dichlorophenol, and triclosan, respectively. The precision expressed as the relative standard deviation ranged from 2.20% to 5.04% for spiked water at 10 µg · L ^?1 (n = 5) and the fiber to fiber reproducibility was between 3.27% and 5.91% (n = 5). The method was successfully applied to the determination of chlorophenolics in real water samples. The recoveries of chlorophenolics in spiked water at 5.0 µg · L^?1 were between 99.60% and 108.7% with relative standard deviations between 3.24% and 5.47%.     

Multivariate Analysis for the Classification Differentiation of Brazilian Sugarcane Spirits by Analysis of Organic and Inorganic Compounds

Abstract

Brazilian sugarcane spirits were analyzed to elucidate similarities and dissimilarities by principal component analysis. Nine aldehydes, six alcohols, and six metal cations were identified and quantified. Isobutanol (LD 202.9 µg L^?1), butiraldehyde (0.08–0.5 µg L^?1), ethanol (39–47% v/v), and copper (371–6068 µg L^?1) showed marked similarities, but the concentration levels of n-butanol (1.6–7.3 µg L^?1), sec-butanol (LD 89 µg L^?1), formaldehyde (0.1–0.74 µg L^?1), valeraldehyde (0.04–0.31 µg L^?1), iron (8.6–139.1 µg L^?1), and magnesium (LD 1149 µg L^?1) exhibited differences from samples.     

Rheological characterization of functional walnut oil-enriched butters stabilized by the various polysaccharides

Dynamic rheological measurements provide a valid determination of the ability of polymeric ingredients to compensate the reduced contribution of fat to texture and mouthfeel, as well as provide an emulsion that easily breaks down in commercial low-fat butters. In this study, the linear effects of pectin (PE, 0.5%) and xanthan gum (XG, 0.1%) and their interactions with locust bean gum (LBG, 0.2% and 0.4%), sodium-alginate (ALG, 0.2% and 0.4%), and modified starch (MS, 0.2% and 0.4%) on the flow behavior, dynamic rheological characteristics, and stability of reduced-fat butters containing 10% walnut oil (WO) were investigated. Results showed that the power law model can adequately fit the shear-rate/shear-stress data (0.888?≤?r?≤?0.992, p?G′?>?G″ at all frequencies. The samples prepared with PE–LBG (0.2% and 0.4%) and XG–ALG (0.4%) had the highest G′ values. The phase angle (G″/G′) decreased with increasing frequency from 0.03 to 15?Hz. The maximum apparent viscosity and stability were, respectively, found for WO butters formulated with XG–0.2% ALG and PE–0.4% LBG.     

A SPE-LC-MS/MS Method for the Detection of Low Concentrations of Pharmaceuticals in Industrial Waste Streams

A SPE-LC-MS/MS method was developed and validated for the determination of three active pharmaceutical ingredients [API A (3-([2-(diaminomethyleneamino)thiazol-4-yl]methylthio)-N′-sulfamoyl propanimid amide, API B 5-[(2 R)-2-[2-(2-ethoxyphenoxy)ethylamino]propyl]-2-methoxybenzenesulfonamide hydrochloride, API C 1-azabicyclo[2.2.2]octan-8-yl (1S)-1-phenyl-3,4-dihydro-1H-isoquinoline-2-carboxylate] in the wastewater of a chemical synthesis production facility. The SPE-LC-MS/MS method was validated in actual influent and effluent samples. Linearity, LOD, LOQ, repeatability, intermediate precision, and recovery were determined. An LOQ of 400 μg · L^?1, 1.0 μg · L^?1, and 6 μg · L^?1, repeatability of 2.5% CV, 14.8% CV, and 11.9% CV, intermediate precision of 7.8% CV, 11.0% CV, and 8.7% CV and SPE recovery of 114%, 103%, and 91% was determined for API A, B, and C, respectively, in influent. An LOQ of 400 μg · L^?1, 0.8 μg · L^?1, and 6 μg · L^?1, repeatability of 2.0% CV, 11.0% CV, and 10.9% CV, intermediate precision of 1.7% CV, 6.8% CV, and 10.2% CV and SPE recovery of 116%, 96%, and 115% was established for API A, B, and C, respectively, in effluent. Coefficients of correlation for each analyte were >0.9301 confirming the linearity of the method. The LC-MS/MS method was used for an on-going monitoring program for these pharmaceuticals in wastewater. The method development techniques, validation procedures, and results from real wastewater samples are presented in this paper.     

Use of ionic liquid based chitosan as sorbent for preconcentration of fluoroquinolones in milk,egg, fish,bovine, and chicken meat samples by solid phase extraction prior to HPLC determination

The possibility of using ionic liquid based chitosan sorbent for the separation and preconcentration of fluoroquinolone antibiotics (marbofloxacin, enoxacin, ofloxacin, ciprofloxacin, and enrofloxacin) has been studied. For this reason, different ionic liquids were prepared and coated on the chitosan sorbent. The conditions of the preconcentration of fluoroquinolones on a microcolumn have been optimized and the extraction efficiencies of the prepared sorbents have been compared. The compounds were eluted with 5 mL of 20% NH₃ (v/v, MeOH) solution and determined by HPLC with diode array and fluorescence detector. The limits of detection were found as 4.23 µ g L^?1 for marbofloxacin, and 1.09 µg L^?1 for enoxacin; 3.23 × 10^?3 µg L^?1 for ofloxacin; 8.39 × 10^?3 µg L^?1 for ciprofloxacin; and 19.50 × 10^?3 µg L^?1 for enrofloxacin. The developed method was applied for the analysis of fluoroquinolone in milk, egg, fish, bovine, and chicken samples and the recoveries were obtained in the range 70–100%.     

Rheological and microrheological characterization of a novel amphoteric xanthan gum

A novel amphoteric xanthan gum (AXG) containing anionic carboxyl groups and cationic quaternary ammonium substituents was prepared from xanthan gum (XG) and 3-chloro-2-hydroxypropyltriethanolammonium acetate. The rheological and microrheological properties of AXG and XG solutions were studied in this work. The rheological results showed that the apparent viscosity of the 0.4% AXG solution was 5.26 times that of the 0.4% XG solution, and the AXG solution exhibited more obvious thixotropy and much stronger viscoelasticity than the XG solution. Both experiment and numerical simulations were adopted to investigate the gel-breaking process of the AXG solution, and the rheokinetics equations can well describe the evolution of complex viscosity. Moreover, the optical microrheology method was also adopted to investigate the microrheological behavior of AXG and XG solutions. The microrheological results showed that the AXG solution exhibited higher viscosity index at zero shear and a more obvious solid-like behavior than the XG solution. Good agreement is found when comparing the results obtained from microrheology to classical rheology, which verifies the feasibility of the microrheology method for measuring the solution properties, especially some properties not well described by the current rheological approach.     

Single Laboratory Validation of a Method for the Determination of Total Inorganic Arsenic by Hydride Generation Atomic Absorption Spectrometry

The purpose of this study consists in reporting of single laboratory validation of a method for the determination of total inorganic arsenic by hydride generation atomic absorption spectrometry from natural and residual water samples. Applicability, fitness for purpose, selectivity, and sensitivity were discussed. A calibration study was realized, linear working range (0.4–4 μg·L^?1), detection (0.11 μg·L^?1), and quantification (0.38 μg·L^?1) limits being determined. It was also proven that the method is accurate and precise. Following the bottom-up approach measurement, uncertainty was estimated (method validation data were used).     

Trace Determination of Manganese in Urine by Graphite Furnace Atomic Absorption Spectrometry and Inductively Coupled Plasma–Mass Spectrometry

This paper describes a simple and sensitive method for the determination of manganese in human urine by graphite furnace atomic absorption spectroscopy (GFAAS), which includes sample preparation by microwave digestion. Matrix modifier combinations, the digestion power, pyrolysis, and atomization temperatures were optimized. A mixture of 5.0 µg Pd(NO₃)₂ and 3.2 µg Mg(NO₃)₂ modifier presented the best performance. The optimal temperatures for pyrolysis and atomization were 1500°C and 1950°C, respectively. The GFAAS method was compared to inductively coupled plasma–mass spectrometry (ICP–MS) for the determination of manganese in urine. Analytical figures of merit for GFAAS and ICP–MS were: accuracy (3.46%, 2.19%), precision (3.61%, 5.84%), LOD (0.109 µg · L^?1, 0.015 µg · L^?1), LOQ (0.327 µg · L^?1, 0.045 µg · L^?1), and recovery (80–100%, 74–89%). Both methods were employed for the determination of Mn in urine and the results were compared statistically.     

Determination of Organotin Compounds in Wine by Microwave-Assisted Extraction and High Performance Liquid Chromatography–Inductively Coupled Plasma Mass Spectrometry

A new analytical procedure for the determination of five organotin compounds in several matrix wine samples is reported. The organotin compounds were extracted by microwave-assisted extraction with n-hexane. Extraction conditions, such as volume of n-hexane required, extraction temperature, and extraction time, were investigated and optimized by an orthogonal array experimental design. The determination of organotin compounds in the final extracts was carried out by liquid chromatography–inductively coupled plasma mass spectrometry. The procedure showed limits of detection between 0.029–0.049 µg · L^?1. The linearity was in the range of 0.5 to 100 µg · L^?1. The precision expressed as relative standard deviation (RSD) was below 9.43%. The developed method was successfully employed to analyze different matrix wine samples, and some analytes were detected at the level of 0.053 to 1.14 µg · L^?1.     

Co-gelation mechanism of xanthan and galactomannan

Synergistic gelation of dilute (0.1% total gums) mixed solutions of xanthan and galactomannan isolated from seeds of Delonix regia was investigated. Gelation occurred in a mixed solution of xanthan and galactomannan at 0.1% total gums at room temperature (25 °C). The flow curves of mixed solutions of native xanthan and galactomannan showed plastic behavior. The maximum elastic modulus was obtained when the ratio of the xanthan to galactomannan was 2:1 at room temperature (25 °C). The largest elastic modulus was observed in the mixture solution of deacetylated xanthan. However, a small elastic modulus was obtained in the mixture with depyruvated xanthan. The results obtained supported the interaction mechanism between xanthan and galactomannan (locust bean gum) previously proposed, and the pyruvate methyl groups might also take part in the interaction.     

Phase formation and transition in a xanthan gum/H2O/H3PO4 tertiary system

Phase formation and transition in a xanthan gum (XG)/H₂O/H₃PO₄ tertiary system were characterized by polarized optical microscopy, light transmission detection and rheological methods. Three distinct phases and a transition region—the completely separated (S) phase, the liquid crystalline (LC) miscible phase, the isotropically (I) miscible phase and the S plus LC region—were identified. The presence of H₃PO₄ in the XG/H₂O system inhibited the evolution of both the S and LC phases. The S and LC phases contained less than 73 and 62 wt% of H₃PO₄, respectively. As the temperature increased over 65 °C, the LC phase in the H₃PO₄-rich and H₂O-poor region seriously shrunk owing to the breakup of hydrogen bonds among the XG helical structure. At the same XG loading, the viscosity of the XG solutions in LC phase was found to be much higher than that in I phase. It indicated the existence of numerous XG intermolecular interactions in the LC phase that suppress the movement of liquid. A study of the kinetics demonstrated that the shrinkage relaxation time (τ) depended strongly on temperature and was fitted by the Volgel-Fulcher-Tammann (VFT) expression. The potential energy barrier of this liquid was quite low at approximately 3.0 kJ mol^?1, falling in the range of hydrogen-bond disassociation. The light absorbance test in heating mode revealed a biphasic transitional region between the LC phase and I phase. The contour of this region depended on the heating rate, and this fact was explained again by the relaxation behavior of XG helices at temperatures higher than 65 °C.     

Speciation and determination of chromium ions by dispersive micro solid phase extraction using magnetic graphene oxide followed by flame atomic absorption spectrometry

A selective, simple and fast dispersive micro solid phase extraction method using magnetic graphene oxide (GO) as an efficient sorbent has been developed for the extraction, separation and speciation analysis of chromium ions. The method is based on different adsorption behaviour of Cr(VI) and Cr(III) species onto magnetic GO in aqueous solutions which allowed the selective separation and extraction of Cr(VI) in the pH range of 2.0–3.0. The retained Cr(VI) ions by the sorbent were eluted using 0.5 mL of 0.5 mol L^?1 nitric acid solution in methanol and determined by ?ame atomic absorption spectrometry. Total chromium content was determined after the oxidation of Cr(III) to Cr(VI) by potassium permanganate. All effective parameters on the performance of the extraction process were thoroughly investigated and optimised. Under the optimised conditions, the method exhibited a linear dynamic range of 0.5–50.0 µg L^?1 with a detection limit of 0.1 µg L^?1 and pre-concentration factor of 200. The relative standard deviations of 3.8% and 4.6% (n = 8) were obtained at 25.0 µg L^?1 level of Cr(VI) for intra- and inter-day analysis, respectively. The method was successfully applied to the speciation and determination of Cr(VI) and Cr(III) in environmental water samples.     

A stir foam composed of graphene oxide,poly(ethylene glycol) and natural latex for the extraction of preservatives and antioxidant

A stir foam composed of graphene oxide, poly(ethylene glycol) and natural latex (GO-PEG-NL) was prepared for use in micro-solid phase extraction sorbent of preservative agents and antioxidants from cosmetic products. The extracted analytes were quantified by GC-MS. Under the optimized conditions, the calibration plots are linear in the concentration ranges between 5.0 μg·L^?1 to 1.0 mg·L^?1 for benzoic acid, of 10.0 μg·L^?1 to 1.0 mg·L^?1 for 2-methyl-3-isothiazolinone (MI), and between 1.0 μg·L^?1 and 1.0 mg·L^?1 for both 3-tert-butyl-4-hydroxyanisole (BHA) and 2,6-di-tert-butyl-p-hydroxytoluene (BHT). The LODs are 1.0 μg·L^?1 for benzoic acid, 5.0 μg·L^?1 for MI and 0.5 μg·L^?1 for both BHA and BHT. The stir-foam can be easily prepared, is inexpensive and well reproducible (RSDs <3%, for n?=?6). It can be re-used for up to 12 times after which extraction efficiency has dropped to 90%. The method was successfully applied to the determination of preservatives and antioxidants in cosmetic samples. Recoveries from spiked samples ranged between 94.5?±?2.1% and 99.8?±?1.8%.

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Graphical abstract A stir foam was prepared from graphene oxide, poly(ethylene glycol) and natural latex (GO-PEG-NL) and is shown to be a most viable sorbent for the microextraction of trace amounts of preservative agents and antioxidants from cosmetic products.

     

Generic Automated Fluorimetric Assay for the Quality Control of Gamma Aminobutyric Acid-Analogue Anti-Epileptic Drugs Using Sequential Injection

The first sequential injection assay for the generic determination of gabapentin and pregabalin is reported. The analytes react with o-phthalaldehyde in the presence of N-acetylcysteine as a nucleophilic reagent in alkaline medium under flow conditions to form highly fluorescent derivatives. The effect of the main instrumental and chemical variables on the assay was examined. The proposed method was validated for both analytes in terms of linearity, detection, and quantitation limits (c _L  = 160 μg L^?1, c _Q  = 480 μg L^?1 for gabapentin, and c _L  = 70 μg L^?1, c _Q  = 210 μg L^?1 for pregabalin), precision (s _r  < 1.0% in both cases), selectivity, and accuracy. The applicability of the assay was demonstrated by successfully analyzing commercially available formulations. The experimental percent recoveries were in the range of 97.9–102.0% for gabapentin and 98.3–102.3% for pregabalin.     

Spectrophotometric Determination of Gold in Water and Ore with 2‐Carboxyl‐1‐Naphthalthiorhodanine

Abstract

This paper reports on the synthesis of a new chromogenic reagent, 2‐carboxyl‐1‐naphthalthiorhodanine (CNTR). A high sensitive, selective, and rapid method for the determination of gold based on the rapid reaction of gold with CNTR and the solid phase extraction of the colored chelate with a reversed phase polymer‐based C₁₈ cartridge was developed. In the presence of 0.05–0.5 mol L^?1 of phosphoric acid solution and emulsifier‐OP medium, CNTR reacts with gold to form a red chelate of a molar ratio 1∶3 (gold to CNTR). This chelate was enriched by the solid phase extraction with a polymer‐based C₁₈ cartridge and the retained chelate was eluted from the cartridge with dimethyl formamide (DMF). The enrichment factor of 100 was achieved. In the DMF medium, the molar absorptivity of the chelate is 1.35×10⁵ L · mol^?1 · cm^?1 at 540 nm. Beer's law is obeyed in the range of 0.01～2 µg mL^?1 in the measured solution. The relative standard deviation for 11 replicates sample of 0.5 µg L^?1 level is 2.05%. The detection limit, based on three times the standard deviation is 0.02 µg L^?1 in the original sample. This method was applied to the determination of gold in water and ore with good results.     

Determination of N-methylcarbamate pesticides using flow injection with photoinduced chemiluminescence detection

A sensitive, economic, rapid and simple method for the determination of four N-methylcarbamate pesticides: methomyl (2.0–80 μg L^?1), aldicarb (5.0–50 μg L^?1), butocarboxim (2.0–60 μg L^?1) and oxamyl (2.0–60 μg L^?1); is reported. It relies on the coupling of photoinduced chemiluminescence (PICL) detection with flow injection (FI) methodology. The automation of FI together with the use of light as a reagent decreased the environmental impact of the analysis. The proposed method was based on the oxidation of these pesticides, previously irradiated on-line with UV light, with cerium(IV), using quinine as a sensitiser. Limits of detection below the legal limits (100 ng L^?1) established by the European Union for drinking waters were obtained without the need of preconcentration steps. A good inter-day reproducibility (1.6–6.4%, n = 5), repeatability (rsd = 2.7 %, n = 25) and high throughput (123 h^?1) were achieved. The method was successfully applied to the determination of methomyl in natural waters with mean recoveries ranging from 90% to 98%.