Combined of ultrasound irradiation with high hydrostatic pressure (US/HHP) as a new method to improve immobilization of dextranase onto alginate gel

In this research work, dextranase was immobilized onto calcium alginate beads by the combination of ultrasonic irradiation and high hydrostatic pressure (US/HHP) treatments. Effects of US/HHP treatments on loading efficiency and immobilization yield of dextranase enzyme onto calcium alginate beads were investigated. Furthermore, the activities of immobilized enzymes prepared with and without US/HHP treatments and that prepared with ultrasonic irradiation (US) and high hydrostatic pressure (HHP), as a function of pH, temperature, recyclability and enzyme kinetic parameters, were compared with that for free enzyme. The maximum loading efficiency and the immobilization yield were observed when the immobilized dextranase was prepared with US (40 W at 25 kHz for 15 min) combined with HHP (400 MPa for 15 min), under which the loading efficiency and the immobilization yield increased by 88.92% and 80.86%, respectively, compared to immobilized enzymes prepared without US/HHP treatment. On the other hand, immobilized enzyme prepared with US/HHP treatment showed V_max, K_M, catalytic and specificity constants values higher than that for the immobilized enzyme prepared with HHP treatment, indicated that, this new US/HHP method improved the catalytic kinetics activity of immobilized dextranase at all the reaction conditions studied. Compared to immobilized enzyme prepared either with US or HHP, the immobilized enzymes prepared with US/HHP method exhibited a higher: pH optimum, optimal reaction temperature, thermal stability and recyclability, and lower activation energy, which, illustrating the effectiveness of the US/HHP method. These results indicated that, the combination of US and HHP treatments could be an effective method for improving the immobilization of enzymes in polymers.     

Sonochemical degradation of ethyl paraben in environmental samples: Statistically important parameters determining kinetics,by-products and pathways

The sonochemical degradation of ethyl paraben (EP), a representative of the parabens family, was investigated. Experiments were conducted at constant ultrasound frequency of 20 kHz and liquid bulk temperature of 30 °C in the following range of experimental conditions: EP concentration 250–1250 μg/L, ultrasound (US) density 20–60 W/L, reaction time up to 120 min, initial pH 3–8 and sodium persulfate 0–100 mg/L, either in ultrapure water or secondary treated wastewater.A factorial design methodology was adopted to elucidate the statistically important effects and their interactions and a full empirical model comprising seventeen terms was originally developed. Omitting several terms of lower significance, a reduced model that can reliably simulate the process was finally proposed; this includes EP concentration, reaction time, power density and initial pH, as well as the interactions (EP concentration) × (US density), (EP concentration) × (pH_o) and (EP concentration) × (time).Experiments at an increased EP concentration of 3.5 mg/L were also performed to identify degradation by-products. LC–TOF–MS analysis revealed that EP sonochemical degradation occurs through dealkylation of the ethyl chain to form methyl paraben, while successive hydroxylation of the aromatic ring yields 4-hydroxybenzoic, 2,4-dihydroxybenzoic and 3,4-dihydroxybenzoic acids. By-products are less toxic to bacterium V. fischeri than the parent compound.     

Ultrasound assisted extraction of pectin from waste Artocarpus heterophyllus fruit peel

Four factors three level face centered central composite response surface design was employed in this study to investigate and optimize the effect of process variables (liquid-solid (LS) ratio (10:1–20:1 ml/g), pH (1−2), sonication time (15–30 min) and extraction temperature (50–70 °C)) on the maximum extraction yield of pectin from waste Artocarpus heterophyllus (Jackfruit) peel by ultrasound assisted extraction method. Numerical optimization method was adapted in this study and the following optimal condition was obtained as follows: Liquid-solid ratio of 15:1 ml/g, pH of 1.6, sonication time of 24 min and temperature of 60 °C. The optimal condition was validated through experiments and the observed value was interrelated with predicted value.     

Ultrasonically assisted hydrothermal synthesis of activated carbon–HKUST-1-MOF hybrid for efficient simultaneous ultrasound-assisted removal of ternary organic dyes and antibacterial investigation: Taguchi optimization

Activated carbon (AC) composite with HKUST-1 metal organic framework (AC–HKUST-1 MOF) was prepared by ultrasonically assisted hydrothermal method and characterized by FTIR, SEM and XRD analysis and laterally was applied for the simultaneous ultrasound-assisted removal of crystal violet (CV), disulfine blue (DSB) and quinoline yellow (QY) dyes in their ternary solution. In addition, this material, was screened in vitro for their antibacterial actively against Methicillin-resistant Staphylococcus aureus (MRSA) and Pseudomonas aeruginosa (PAO1) bacteria. In dyes removal process, the effects of important variables such as initial concentration of dyes, adsorbent mass, pH and sonication time on adsorption process optimized by Taguchi approach. Optimum values of 4, 0.02 g, 4 min, 10 mg L⁻¹ were obtained for pH, AC–HKUST-1 MOF mass, sonication time and the concentration of each dye, respectively. At the optimized condition, the removal percentages of CV, DSB and QY were found to be 99.76%, 91.10%, and 90.75%, respectively, with desirability of 0.989. Kinetics of adsorption processes follow pseudo-second-order model. The Langmuir model as best method with high applicability for representation of experimental data, while maximum mono layer adsorption capacity for CV, DSB and QY on AC–HKUST-1 estimated to be 133.33, 129.87 and 65.37 mg g⁻¹ which significantly were higher than HKUST-1 as sole material with Q_m to equate 59.45, 57.14 and 38.80 mg g⁻¹, respectively.     

Combined effect of blanching and sonication on quality parameters of bottle gourd (Lagenaria siceraria) juice

This study evaluated the combined effect of blanching and sonication treatment on selected quality parameters of bottle gourd juice (BGJ). Bottle gourd cubes were blanched and juice was extracted. Effect of frequency (20–50 kHz), amplitude (50–90%) and time (10–30 min) was also studied on quality parameters like titratable acidity (TA), pH, total soluble solids (TSS), physical stability (PS), ascorbic acid (AA), total phenolics (TP), total carotenoids (TC), browning index (BI), total plate count (TPC) and yeast & mold count (Y&M) of BGJ to derive the level of these parameters. Combined effect of blanching followed by sonication (BFS) showed significant (P ⩽ 0.05) change in all quality parameters except TA. Highest percentage of TSS (5.9 °B), PS (2%), AA (18.99 mg/100 g), TP (1010 mg/100 g) and TC (5.8 mg/100 g) was observed at 70% amplitude, 50 kHz frequency and 20 min. Results suggested 70% amplitude, 50 kHz frequency and 20 min as best treatment conditions for processing of BGJ. Microstructure examination, transmission electron microscopy (TEM) and laser diffraction analysis of BGJ showed significant change in particle size and distribution. Moreover, TEM of blanched and sonicated samples of BGJ also showed significant (P ⩽ 0.05) change in microbial profile.     

Investigation on the interactions of silymarin to bovine serum albumin and lysozyme by fluorescence and absorbance

The interactions of silymarin with bovine serum albumin (BSA) and lysozyme (LYS) were investigated in physiological buffer (pH = 7.4) by fluorescence spectroscopy and UV–vis absorption spectroscopy. The mechanism study indicated that silymarin could strongly quench the intrinsic fluorescence of BSA and LYS through static quenching procedures. At 291 K, the values of the binding constant K_A were 4.20×10⁴ and 4.71×10⁴ L mol^?1 for silymarin–BSA and silymarin–LYS, respectively. Using thermodynamic equations, the conclusion that hydrophobic and electrostatic forces played an important role in stabilizing complex of silymarin–BSA or silymarin–LYS was obtained. The effects of Cu²⁺, Mg²⁺, Ca²⁺, Fe²⁺, and Fe³⁺ on the binding were also studied at 291 K. According to Förster’s nonradiative energy transfer theory, the distances r₀ between donor and acceptor were calculated to be 3.36 and 2.71 nm for silymarin–BSA and silymarin–LYS, respectively. Synchronous fluorescence spectra showed that the conformation of BSA and LYS were changed by silymarin.     

Optimization of a heterogeneous catalytic hydrodynamic cavitation reactor performance in decolorization of Rhodamine B: Application of scrap iron sheets

A low pressure pilot scale hydrodynamic cavitation (HC) reactor with 30 L volume, using fixed scrap iron sheets, as the heterogeneous catalyst, with no external source of H₂O₂ was devised to investigate the effects of operating parameters of the HC reactor performance. In situ generation of Fenton reagents suggested an induced advanced Fenton process (IAFP) to explain the enhancing effect of the used catalyst in the HC process. The reactor optimization was done based upon the extent of decolorization (ED) of aqueous solution of Rhodamine B (RhB). To have a perfect study on the pertinent parameters of the heterogeneous catalyzed HC reactor, the following cases as, the effects of scrap iron sheets, inlet pressure (2.4–5.8 bar), the distance between orifice plates and catalyst sheets (submerged and inline located orifice plates), back-pressure (2–6 bar), orifice plates type (4 various orifice plates), pH (2–10) and initial RhB concentration (2–14 mg L^?1) have been investigated. The results showed that the highest cavitational yield can be obtained at pH 3 and initial dye concentration of 10 mg L^?1. Also, an increase in the inlet pressure would lead to an increase in the ED. In addition, it was found that using the deeper holes (thicker orifice plates) would lead to lower ED, and holes with larger diameter would lead to the higher ED in the same cross-sectional area, but in the same holes’ diameters, higher cross-sectional area leads to the lower ED. The submerged operation mode showed a greater cavitational effects rather than the inline mode. Also, for the inline mode, the optimum value of 3 bar was obtained for the back-pressure condition in the system. Moreover, according to the analysis of changes in the UV–Vis spectra of RhB, both degradation of RhB chromophore structure and N-deethylation were occurred during the catalyzed HC process.     

The collagen type I segment long spacing (SLS) and fibrillar forms: Formation by ATP and sulphonated diazo dyes

The collagen type I segment long spacing (SLS) crystallite is a well-ordered rod-like molecular aggregate, ∼300 nm in length, which is produced in vitro under mildly acidic conditions (pH 2.5–3.5) in the presence of 1 mM ATP. The formation of the SLS crystallite amplifies the inherent linear structural features of individual collagen heterotrimers, due to the punctate linear distribution and summation of the bulkier amino acid side chains along the length of individual collagen heterotrimers. This can be correlated structurally with the 67 nm D-banded collagen fibril that is found in vivo, and formed in vitro. Although first described many years ago, the range of conditions required for ATP-induced SLS crystallite formation from acid-soluble collagen have not been explored extensively. Consequently, we have addressed biochemical parameters such as the ATP concentration, pH, speed of formation and stability so as to provide a more complete structural understanding of the SLS crystallite. Treatment of collagen type I with 1 mM ATP at neutral and higher pH (6.0–9.0) also induced the formation of D-banded fibrils. Contrary to previous studies, we have shown that the polysulphonated diazo dyes Direct red (Sirius red) and Evans blue, but not Congo red and Methyl blue, can also induce the formation of SLS-like aggregates of collagen, but under markedly different ionic conditions to those employed in the presence of ATP. Specifically, pre-formed D-banded collagen fibrils, prepared in a higher than the usual physiological NaCl concentration (e.g. 500 mM NaCl, 20 mM Tris-HCl pH7.4 or x3 PBS), readily form SLS aggregates when treated with 0.1 mM Direct red and Evans blue, but this did not occur at lower NaCl concentrations. These new data are discussed in relation to the anion (Cl⁻) and polyanion (phosphate and sulphonate) binding by the collagen heterotrimer and their likely role in collagen fibrillogenesis and SLS formation.     

Ultrasonic degradation of acetaminophen in water: Effect of sonochemical parameters and water matrix

This paper deals about the sonochemical water treatment of acetaminophen (ACP, N-acetyl-p-aminophenol or paracetamol), one of the most popular pharmaceutical compounds found in natural and drinking waters. Effect of ultrasonic power (20–60 W), initial ACP concentration (33–1323 μmol L⁻¹) and pH (3–12) were evaluated. High ultrasonic powers and, low and natural acidic pH values favored the efficiency of the treatment. Effect of initial substrate concentration showed that the Langmuir-type kinetic model fit well the ACP sonochemical degradation. The influence of organic compounds in the water matrix, at concentrations 10-fold higher than ACP, was also evaluated. The results indicated that only organic compounds having a higher value of the Henry’s law constant than the substrate decrease the efficiency of the treatment. On the other hand, ACP degradation in mineral natural water showed to be strongly dependent of the initial substrate concentration. A positive matrix effect was observed at low ACP concentrations (1.65 μmol L⁻¹), which was attributed to the presence of bicarbonate ion in solution. However, at relative high ACP concentrations a detrimental effect of matrix components was noticed. Finally, the results indicated that ultrasonic action is able to transform ACP in aliphatic organic compounds that could be subsequently eliminated in a biological system.     

Optimization of ultrasound-assisted dispersive solid-phase microextraction based on nanoparticles followed by spectrophotometry for the simultaneous determination of dyes using experimental design

A simple, low cost and ultrasensitive method for the simultaneous preconcentration and determination of trace amount of auramine-O and malachite green in aqueous media following accumulation on novel and lower toxicity nanomaterials by ultrasound-assisted dispersive solid phase micro-extraction (UA-DSPME) procedure combined with spectrophotometric has been described. The Mn doped ZnS nanoparticles loaded on activated carbon were characterized by Field emission scanning electron microscopy (FE-SEM), particle size distribution, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) analyses and subsequently were used as green and efficient material for dyes accumulation. Contribution of experimental variables such as ultrasonic time, ultrasonic temperature, adsorbent mass, vortex time, ionic strength, pH and elution volume were optimized through experimental design, and while the preconcentrated analytes were efficiently eluted by acetone. Preliminary Plackett–Burman design was applied for selection of most significant factors and giving useful information about their main and interaction part of significant variables like ultrasonic time, adsorbent mass, elution volume and pH were obtained by central composite design combined with response surface analysis and optimum experimental conditions was set at pH of 8.0, 1.2 mg of adsorbent, 150 μL eluent and 3.7 min sonication. Under optimized conditions, the average recoveries (five replicates) for two dyes (spiked at 500.0 ng mL⁻¹) changes in the range of 92.80–97.70% with acceptable RSD% less than 4.0% over a linear range of 3.0–5000.0 ng mL⁻¹ for the AO and MG in water samples with regression coefficients (R²) of 0.9975 and 0.9977, respectively. Acceptable limits of detection of 0.91 and 0.61 ng mL⁻¹ for AO and MG, respectively and high accuracy and repeatability are unique advantages of present method to improve the figures of merit for their accurate determination at trace level in complicated materials.     

Ultrastructure of antennal sensilla of an autoparasitoid Encarsia sophia (Hymenoptera: Aphelinidae)

Encarsia sophia (Hymenoptera: Aphelinidae) is a parasitoid utilized for biological control of Bemisia tabaci, with selection of prey aided by chemoreceptor organs. The morphology and distribution of the antennal sensilla (chemoreceptors) of E. sophia were examined using Transmission electron micrographs. The total antennal length for E. sophia was 429.28 ± 0.95 μm for females and 437.19 ± 8.21 for males, and each antennae was found to consist of seven sensilla of different types. Both sexes possessed sensilla chaetica, sensilla trichodea, basiconic capitate peg sensilla, multiporous grooved-surface placoid sensilla (MG-PS), uniporous rod-like sensilla, nonporous finger-like sensilla, and sensilla coeloconica. Transmission electron micrographs of longitudinal sections of female antennae showed that they were composed of fat body, cuticle, mesoscutello-metanotal muscles, neurons, and glandular tissue, and cross-sections of the basal MG-PS showed sensillar lymph cavities and dendrites. The MG-PSs were imbedded in an electron-dense mass with cuticular invaginations which acted as pores that connected to a central lumen. The possible function of each type of sensilla is discussed.     

Cathodoluminescence studies of un-doped and (Cu,Fe, and Co)-doped tin dioxide films deposited by spray pyrolysis

Un-doped and (Cu, Fe, and Co)-doped SnO₂ were studied using films deposited by spray pyrolysis. Room temperature cathodoluminescence (CL) was measured. Differences in CL spectra were observed as a function of deposition parameters (T_sub-350–550 °C), the nature and concentration of dopants (0–16 at.%), and the resulting high annealing temperature (T_an = 700–950 °C). A possible luminescence mechanism has been discussed. It was established that changes taking place in CL spectra were caused by the change of both the grain size and crystallinity (stoichiometry) of the surface layer. It was concluded that radiative recombination occurs through shallow donor levels associated with O-vacancies and trapped centers. It was assumed that in SnO₂ there are apparently three types of defects forming deep levels located at 0.8–0.9, 1.3–1.4, and ∼1.6 eV from the top of the valence band.     

Application of ZnO nanorods loaded on activated carbon for ultrasonic assisted dyes removal: Experimental design and derivative spectrophotometry method

A method based on application of ZnO nanorods loaded on activated carbon (ZnO-NRs-AC) for adsorption of Bromocresol Green (BCG) and Eosin Y (EY) accelerated by ultrasound was described. The present material was synthesized under ultrasound assisted wet-chemical method and subsequently was characterized by FE-SEM, TEM, BET and XRD analysis. The extent of contribution of conventional variables like pH (2.0–10.0), BCG concentration (4–20 mg L⁻¹), EY concentration (3–23 mg L⁻¹), adsorbent dosage (0.01–0.03 g), sonication time (1–5 min) and centrifuge time (2–6 min) as main and interaction part were investigated by central composite design under response surface methodology. Analysis of variance (ANOVA) was adapted to experimental data and guide the best operational conditions mass by set at 6.0, 9 mg L⁻¹, 10 mg L⁻¹, 0.02 g, 4 and 4 min for pH, BCG concentration, EY concentration, adsorbent dosage, sonication and centrifuge time, respectively. At these specified conditions dye adsorption efficiency was higher than 99.5%. The suitability and well prediction of optimum point was tested by conducting five experiments and respective results revel that RSD% was lower than 3% and high quality of fitting was confirmed by t-test. The experimental data were best fitted in Langmuir isotherm equation and the removal followed pseudo second order kinetics. The experimentally obtained maximum adsorption capacities were estimated as 57.80 and 61.73 mg g⁻¹ of ZnO-NRs-AC for BCG and EY respectively from binary dye solutions. The mechanism of removal was explained by boundary layer diffusion via intraparticle diffusion.     

Effects of various factors of ultrasonic treatment on the extraction recovery of drugs from fish tissues

In the present research, a combined extraction method of ultrasound-assisted extraction (UAE) in conjunction with solid phase extraction (SPE) was applied to isolation and enrichment of selected drugs (metoprolol, ticlopidine, propranolol, carbamazepine, naproxen, acenocumarol, diclofenac, ibuprofen) from fish tissues. The extracted analytes were separated and determined by ultra-high performance liquid chromatography with UV detection (UHPLC–UV) technique. The selectivity of the developed UHPLC–UV method was confirmed by comparison with ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) analysis.The important parameters, such as composition of type and pH of extraction solvent, solid/liquid rate volume of extraction solvent and number of extraction cycles were studied. The ultrasonic parameters, such as time, power and temperature of the process were optimized by using a half-fraction factorial central composite design (CCD). The mixture of 10 mL of methanol and 7 mL of water (pH 2.2) (three times) was chosen for the extraction of selected drug from fish tissues. The results showed that the highest recoveries of analytes were obtained with an extraction temperature of 40 °C, ultrasonic power of 300 W, extraction time of 30 min.Under the optimal conditions, the linearity of method was 0.12–5.00 μg/g. The determination coefficients (R²) were from 0.979 to 0.998. The limits of detection (LODs) and limits of quantification (LOQs) for the extracted compounds were 0.04–0.17 μg/g and 0.12–0.50 μg/g, respectively. The recoveries were between 85.5% and 115.8%.     

Estimation of triglycerides by a porous silicon based potentiometric biosensor

A novel, enzymatic, porous silicon (PS) based potentiometric method for estimating triglycerides is reported. Lipase, an enzyme, which hydrolyses triglycerides was immobilised on PS which was prepared from p-type (1 0 0) crystalline silicon and was thermally oxidized. On hydrolysis the triglycerides result in the formation of fatty acids which causes a change in the pH of the solution. Enzyme solution-oxidized PS–crystalline silicon structure was used to detect changes in pH during the hydrolysis of tributyrin as a shift in the capacitance–voltage (C–V) characteristics. Optimisation of the conditions for the enzymatic reaction and calibration of the sensor are included.     

Sonochemical reactions with mesoporous alumina

Herein, we report the sonochemical reactions with MSU-X mesoporous alumina (m-Al₂O₃) in aqueous solutions. Sonication (f = 20 kHz, I = 30 W cm^?2, W_aq = 0.67 W mL^?1, T = 36–38 °C, Ar) causes significant acceleration of m-Al₂O₃ dissolution in the pH range of 4–11. Moreover, power ultrasound has a dramatic effect on the textural properties and phase composition of m-Al₂O₃. Short-time sonication at pH = 4 leads to the formation of nanorods and nanofibers of boehmite, AlO(OH). Prolonged ultrasonic treatment causes high aspect morphology transformation to aggregated nanosheets in weakly acid solutions or plated nanocrystals in alkaline solutions. Sonochemical products in alkaline medium are composed principally from boehmite and small amounts of bayerite, Al(OH)₃. Silent hydrolysis of m-Al₂O₃ yields boehmite at pH = 4 and bayerite at pH = 11. The effect of ultrasound on the textural properties of mesoporous alumina as well as on the transformation of nanosized bayerite to boehmite can be consistently attributed to the transient strong heating of the liquid shell surrounding the cavitation bubble which caused the chemical processes similar to those occurred during hydrothermal treatment.     

Intravoxel incoherent motion diffusion-weighted imaging as an adjunct to dynamic contrast-enhanced MRI to improve accuracy of the differential diagnosis of benign and malignant breast lesions

PurposeTo investigate the value of use of intravoxel incoherent motion diffusion-weighted imaging (IVIM-DWI) as an adjunct to dynamic contrast-enhanced magnetic resonance imaging (DCE-MRI) to distinguish benign from malignant breast lesions.Materials and methodsRetrospective analysis of data pertaining to 117 patients with breast lesions who underwent DCE-MRI and IVIM-DWI examination with 3.0 T MRI was conducted. A total of 128 lesions were pathologically confirmed (47 benign and 81 malignant). Between-group differences in DCE-MRI parameters (Morphology, enhancement pattern, maximum slope of increase (MSI) and time–signal curve (TIC) type) and IVIM-DWI parameters (f value, D value and D* value) were assessed. Multivariate logistic regression was performed to identify variables that distinguished benign from malignant breast lesions. The diagnostic performance of DCE-MRI and DCE-MRI plus IVIM-DWI, to distinguish benign from malignant breast lesions, was evaluated using pathology results as the gold standard.ResultsLesion morphology, MSI, and TIC type (P < 0.05), but not the enhancement pattern (P > 0.05), were significantly different between the benign and malignant groups. The f (8.53 ± 2.14) and D* (7.64 ± 2.07) values in the malignant group were significantly higher than those in the benign group (7.68 ± 1.97 and 6.83 ± 2.13, respectively), while the D value (0.99 ± 0.22) was significantly lower than that (1.34 ± 0.17) in the benign group (P < 0.05 for all). On logistic regression analysis, the sensitivity, specificity and accuracy of DCE-MRI were 90.1%, 70.2% and 82.8% respectively; the corresponding figures for the combination of IVIM-DWI and DCE-MRI were 88.8%, 85.1%, and 87.5%respectively.ConclusionIVIM-DWI method as an adjunct to DCE-MRI can improve the specificity and accuracy in differential diagnosis of benign and malignant lesions of breast.     

Formation of nickel and nickel,zinc-bearing ferrite in aqueous suspension by air oxidation

Stoichiometric Ni-bearing ferrite was formed by air oxidation of an iron(II) hydroxide suspension at an initial Ni : Fe_tot mol ratio (r_Ni) of 0.20 : 2.80 at pH 10.0 and 65°C. Most of products formed at r_Ni=0.40 : 2.60 and 0.60 : 2.40 were Ni-bearing ferrites, of which vacancies of Fe³⁺ ion on the lattice points may be considered. Only Ni, Zn-bearing ferrites were formed in the suspensions at initial (Ni + Zn)  : Fe_tot mol ratios (r_{Ni + Zn}) of 0.20 : 2.80–0.60 : 2.40 at pH 10.0 and 65°C. At higher r_Ni or r_{Ni + Zn} by-products containing Ni, Fe and O₄²⁻ were formed. The formation of the by-products was depressed in the suspensions containing chloride ions in the place of sulfate ions.     

Ultrasound assisted combined molecularly imprinted polymer for selective extraction of nicotinamide in human urine and milk samples: Spectrophotometric determination and optimization study

Ultrasound-assisted dispersive solid phase microextraction followed by UV–vis spectrophotometer (UA-DSPME-UV–vis) was designed for extraction and preconcentration of nicotinamide (vitamin B₃) by HKUST-1 metal organic framework (MOF) based molecularly imprinted polymer (MIP). This new material was characterized by FTIR and FE-SEM techniques. The preliminary Plackett–Burman design was used for screening and subsequently the central composite design justifies significant terms and possible construction of mathematical equation which give the individual and cooperative contribution of variables like HKUST-1-MOF-NA-MIP mass, sonication time, temperature, eluent volume, pH and vortex time. Accordingly the optimum condition was set as: 2.0 mg HKUST-1-MOF-NA-MIP, 200 μL eluent and 5.0 min sonication time in center points other variables were determined as the best conditions to reach the maximum recovery of the analyte. The UA-DSPME-UV–vis method performances like excellent linearity (LR), limits of detection (LOD), limits of quantification of 10–5000 μg L⁻¹ with R² of 0.99, LOD (1.96 ng mL⁻¹), LOQ (6.53 μg L⁻¹), respectively show successful and accurate applicability of the present method for monitoring analytes with within- and between-day precision of 0.96–3.38%. The average absolute recoveries of the nicotinamide extracted from the urine, milk and water samples were 95.85–101.27%.     

Structure relates to elastic recoil and functional role in quadriceps tendon and patellar ligament

Tendons and ligaments have similar but slightly different structure and composition. Crimps of tendons and ligaments are morphological structures related to the elastic functional properties of these connective tissues. Aim of this study was to investigate the morphological arrangement of collagen fibres, fibrils and crimping pattern of suprapatellar (rectus femoris tendon-RFT and vastus intermedius tendon-VIT) and infrapatellar connective tissues (patellar ligament-PL) to relate their structural aspects to their common function role of leg extension. RFT, VIT and PL were removed from knees of Sprague–Dawley rats and light and electron microscopy (TEM and SEM) performed. Sagittal sections showed that collagen array and crimping pattern were similar in RFT and PL but differed from VIT. Morphometric analysis confirmed that crimp number was about the same in RFT and PL (5.4 ± 1.4 and 6.1 ± 2.8 respectively), but it was almost three times higher in VIT (14.5 ± 4.7). Similarly crimp top angle in RFT and PL (141.5 ± 15.0° and 146.2 ± 12.2° respectively) was significantly higher than in VIT (122.3 ± 14.8°) and the crimp base length was more than twice as wide in RFT (75.5 ± 22.6 μm) and PL (72.3 ± 28.9 μm) than in VIT (36 ± 14.1 μm). The smaller, fewer and most crimped crimps in VIT show that this tendon has a greater elastic recoil and responds to higher forces as among quadriceps muscles the vastus intermedius belly contributes the most during knee extension. By contrast, RFT acting as a “stopper” tendon also plays a ligament role by limiting an excessive flexion of the joint during postural rest position of the knee.