Preparation and characterization of astaxanthin-loaded microcapsules and its application in effervescent tablets.

BACKGROUND: Astaxanthin is a type of keto-carotene with potential health benefits. However, astaxanthin has poor solubility and stability, resulting in its low oral bio-availability. Microcapsules can be used to improve the water solubility, stability and oral bio-availability of lipophilic bioactive compounds. Effervescent tablets can further improve the stability, smell and taste of microcapsules, and are more easily accepted by consumers. RESULTS: Astaxanthin-loaded microcapsules were prepared by layer-by-layer assembly and freeze-drying technologies. Sodium caseinate and κ-carrageenan were applied as wall materials. The prepared microcapsules had good flow properties and encapsulation efficiencies (> 85%). Fourier transform infrared spectroscopy demonstrated that the mechanisms of layer-by-layer self-assembly between sodium caseinate and κ-carrageenan might be electrostatic adsorption and hydrogen bonding. The preparation process and excipients did not affect the antioxidant effect of astaxanthin. The in vitro simulated digestion study showed that microcapsules were mainly dissolved and digested in the simulated intestinal solution. Compared with its raw material, microencapsulation could improve the bio-accessibility of astaxanthin greatly. Then, astaxanthin-loaded microcapsules were incorporated into effervescent tablets by wet granulation and tablet-pressing methods. The dissolution of astaxanthin from effervescent tablets was over 90% in 2 h, which indicated a good dissolution effect. A cytotoxicity study revealed that astaxanthin loaded effervescent tablets had a good biocompatibility. Encapsulating astaxanthin-loaded microcapsules in effervescent tablets can improve its chemical stability. CONCLUSION: Effervescent tablets containing microcapsules could be used to improve the solubility, stability and bio-accessibility of lipophilic bioactive compounds. © 2022 Society of Chemical Industry.

Simultaneous determination of five phthalate esters and bisphenol A in milk by packed-nanofiber solid-phase extraction coupled with gas chromatography and mass spectrometry.

A novel polystyrene/pyridine composite nanofiber was synthesized and utilized as the sorbent material for the solid-phase extraction of bisphenol A and five common phthalate esters in milk. The method of extraction integrated extraction and preconcentration of target analytes into a single step. Bisphenol A and five common phthalate esters were selected as target compounds for the development and evaluation of the method. The effects of operating parameters for nanofiber-based solid-phase extraction, such as selection and amount of sorbent, the volume fraction of perchlorate (precipitate protein), desorption solvent, volume of desorption solvent, and effect of salt addition were optimized. Under optimal conditions, higher extraction recoveries (89.6-118.0%) of the six compounds in milk spiked at three levels were obtained, and the satisfied relative standard deviation were ranged from 0.6 to 10.9%. The detection limits and quantification limits of the method ranged from 0.01 to 0.06 µg/L and 0.05 to 0.53 µg/L, respectively. Matrix effects were also verified and well controlled in the range of 91.3-109.3%. The new method gave better performance metrics than Chinese standard method and other published methods. Thus, the proposed method may be applied to the analysis of the phthalate esters and bisphenol A in complex matrixes.

Fabrication and characterization of dihydromyricetin-loaded microcapsules stabilized by glyceryl monostearate and whey protein-xanthan gum.

Dihydromyricetin (DMY) is a lipophilic nutrient with various potential health benefits; however, its poor storage stability and low solubility and bioavailability limit its applications. This study aims to encapsulate DMY in microcapsules by membrane emulsification and freeze-drying methods to overcome these issues. Glyceryl monostearate (GMS, solid lipid) and octyl and decyl glycerate (ODO, liquid lipid) were applied as the inner cores. Whey protein and xanthan gum (XG) were used as wall materials. The prepared microcapsules had an irregular blocky aggregated structure with rough surfaces. All the microcapsules had a DMY loading of 0.85 %-1.1 % and encapsulation efficiency (EE) >85 %. GMS and XG increased the DMY loading and EE. The addition of GMS and an increased XG concentration led to a decrease in the rehydration rate. The in vitro release and digestion studies revealed that GMS and XG controlled the release and digestion of DMY. The chemical stability results indicated that GMS and XG protected DMY against oxidation. An antioxidant capacity study showed that GMS and XG helped DMY in the microcapsules exert antioxidant effects. This research study provides a platform for designing microcapsules with good stability and high bioavailability to deliver lipophilic bioactive compounds.

Coenzyme Q10-loaded microcapsules stabilized by glyceryl monostearate and soy protein isolates-flaxseed gum: Characterization, in vitro release and digestive behavior.

This study aimed to stabilize microcapsules with core materials of glyceryl monostearate (GMS) and octyl and decyl glycerate, and wall materials of soy protein isolates (SPI) and flaxseed gum (FG) by complex coacervation method to overcome the drawbacks of coenzyme Q10 (CoQ10). It was demonstrated by the study that the obtained microcapsules were irregular aggregates. Differential scanning calorimetry and x-ray diffraction patterns indicated that CoQ10 was entrapped inside the disordered semisolid cores of microcapsules. The CoQ10 loading and encapsulation efficiency analysis revealed that GMS and FG helped CoQ10 better encapsulated inside the microcapsules. The in vitro release curve showed a "burst" release of CoQ10 absorbed on the surface of microcapsules for the first 180 min, followed by a sustained release of the encapsulated CoQ10. GMS and FG contributed to the sustained release and the release mechanism of the microcapsules was Fickian diffusion. The in vitro simulated digestion demonstrated that the constructed microcapsules improved the bio-accessibility of CoQ10. Finally, due to the protection of GMS and FG, microcapsules had good storage stability. In conclusion, this study emphasized the potential of using new microcapsules to deliver and protect lipophilic ingredients, providing valuable information for developing functional foods with higher bioavailability.

A novel extraction method for three ochratoxins in human urine based on polystyrene/polyethersulfone electrospun nanofibers coated with copper nanoparticles.

In this study, four types of nanofibers were prepared via electrospinning and characterized through SEM, TEM, EDS, FTIR, TG, XPS and water contact angle analyses, and the novel polystyrene/polyethersulfone nanofibers coated with copper nanoparticles (PS/PES-CuNPs nanofibers) were developed as an ideal adsorbent for the extraction of three ochratoxins from human urine. The solid-phase extractant of sample pretreatment displayed preferable sensitivity and an extraction effect, and the analytical method based on the novel packed-fiber solid-phase extraction strategy followed by high performance liquid chromatography-fluorescence detection (PFSPE-HPLC-FLD) achieved an exceedingly low limit of detection (LOD) and limit of quantification (LOQ) of 0.108-0.162 µg L-1 and 0.658-0.701 µg L-1, respectively; a high spiked recovery of 71.3-92.0% and a lower adsorption time of 7 min, thus demonstrating excellent results compared with other reported adsorbents for ochratoxins from various samples. With the application of this method for the detection of ochratoxins in human urine samples, six in thirty samples were tested positive. This study confirmed that the PS/PES-CuNP nanofibers and PFSPE showed promising potential as a sensitive method for simultaneous extraction and detection of ochratoxins in complex samples.

Preparation and characterization of astaxanthin-loaded microcapsules stabilized by lecithin-chitosan-alginate interfaces with layer-by-layer assembly method.

Astaxanthin is a kind of keto-carotenes with various health benefits. However, its solubility and chemical stability are poor, which leads to low bio-availability. Microcapsules have been reported to improve the solubility, chemical stability, and bio-availability of lipophilic bioactives. Freeze-dried astaxanthin-loaded microcapsules were prepared by layer-by-layer assembly of tertiary emulsions with maltodextrin as the filling matrix. Tertiary emulsions were fabricated by performing chitosan and sodium alginate electrostatic deposition onto soybean lecithin stabilized emulsions. 0.9 wt% of chitosan solution, 0.3 wt% of sodium alginate solution and 20 wt% of maltodextrin were optimized as the suitable concentrations. The prepared microcapsules were powders with irregular blocky structures. The astaxanthin loading was 0.56 ± 0.05 % and the encapsulation efficiency was >90 %. A slow release of astaxanthin could be observed in microcapsules promoted by the modulating of chitosan, alginate and maltodextrin. In vitro simulated digestion displayed that the microcapsules increased the bio-accessibility of astaxanthin to 69 ± 1 %. Chitosan, alginate and maltodextrin can control the digestion of microcapsules. The coating of chitosan and sodium alginate, and the filling of maltodextrin in microcapsules improved the chemical stability of astaxanthin. The constructed microcapsules were valuable to enrich scientific knowledge about improving the application of functional ingredients.

Determination of aflatoxin B1 by novel nanofiber-packed solid-phase extraction coupled with a high performance liquid chromatography-fluorescence detector.

A novel analytical proposal based on nanofiber-packed solid-phase extraction coupled with high performance liquid chromatography-fluorescence detector (HPLC-FLD) has been successfully developed for determining aflatoxin B1 (AFB1) in foods. Four types of nanofibers, including polystyrene (PS) nanofibers, polypyrrole (PPY) nanofibers, polystyrene-acrylic resin (PS-AR) nanofibers, and polystyrene-polyvinyl pyrrolidone (PS-PVP) nanofibers, were fabricated by electrospinning and utilized to prepare a home-made extraction device. In this study, the factors of different fibers, namely, fiber dosage, pH of extraction solution, type of salt ion, concentration of salt ion, and volume of the eluent were optimized. Under optimized conditions, the method showed good linearity in the range of 0.1-40 ng mL-1 with a correlation coefficient greater than 0.999 and good inter-day accuracy (90.8-112.7% recovery) and precision (1.8-3.6% intra-day RSDs, 2.6% inter-day RSD), and the limit of detection (LOD) was 0.05 ng mL-1. Due to its cost-effective, time-saving, environmentally friendly, and simple performance, it has the potential to be utilized to determine aflatoxins in complicated matrices.

The Antioxidant Effect of the Metal and Metal-Oxide Nanoparticles.

Inorganic nanoparticles, such as CeO3, TiO2 and Fe3O4 could be served as a platform for their excellent performance in antioxidant effect. They may offer the feasibility to be further developed for their smaller and controllable sizes, flexibility to be modified, relative low toxicity as well as ease of preparation. In this work, the recent progress of these nanoparticles were illustrated, and the antioxidant mechanism of the inorganic nanoparticles were introduced, which mainly included antioxidant enzyme-mimetic activity and antioxidant ROS/RNS scavenging activity. The antioxidant effects and the applications of several nanoparticles, such as CeO3, Fe3O4, TiO2 and Se, are summarized in this paper. The potential toxicity of these nanoparticles both in vitro and in vivo was well studied for the further applications. Future directions of how to utilize these inorganic nanoparticles to be further applied in some fields, such as medicine, cosmetic and functional food additives were also investigated in this paper.

A novel biosensor based on Blu-ray disc coating film for determination of total amino acid content in tea leaves.

Biosensor substrate materials are a key research focus in the field of sensors. Blu-ray discs (BDs) as universal sensor substrates are advantageous in comparison with other substrates (conventional paper and polycarbonate) in terms of easier activity treatment and higher density of reactive groups on the film surface. In this study, a novel and simple microfluidic biosensor based on BD coating film was developed by treating with sodium hydroxide solution and a piece of filter paper at slightly elevated temperatures. There are no significant physical damages to the substrate morphology, and the aging effect is minimal. The unique wetting, optical, and self-cleaning properties of the modified surfaces can be demonstrated in the paper. We have tested this new type of biosensor substrates for assay applications (the determination of total amino acids in tea leaves), which showed excellent performance in terms of sensitivity and reproducibility. The novel biosensor substrate material based on a simple BD coating film displayed preferable merits with easy making, low cost, easy using, and extensive application prospect.

Adaptive PI Control for Consensus of Multiagent Systems With Relative State Saturation Constraints.

The relative state between neighbors represents the difference of two connected agents' states, and it possesses specific physical meanings in practice. Under this background, the saturation constraints in the relative state inevitably occur. This article studies the consensus problems under the relative state saturation constraints. Novel adaptive proportional-integral (PI) protocols are designed to solve the constrained consensus problem. Specifically, the adaptive coupling weights and the saturation functions are embedded into the proposed protocols, and the former can render the protocols independent of any global topology graph information, while the latter can confine the relative state to stay in its constrained set. Sufficient conditions are identified under which the constrained consensus can be achieved. Considering that the solution matrix is required to be diagonally dominant, an iterative learning-based heuristic algorithm is proposed to seek the diagonally dominant positive-definite solution matrix. For the special case that the input matrix is row full rank, more stringent saturation functions are constructed, and it not only achieves the constrained consensus but also realizes the nonovershoot and shorter settling time associated with edge states. Besides, this result can be applied to preserve connectivity of the communication network. The theoretical analyses are validated by a simulation example.

Nanoparticle-based polyacrylonitrile monolithic column for highly efficient micro solid-phase extraction of carotenoids and vitamins in human serum.

In this work, a biocompatible monolithic column based micro-solid-phase extraction (µ-SPE) method was developed for biological fluid analysis. A novel nanoparticle-based polyacrylonitrile monolithic column (C30 NP-PMC) was fabricated by incorporating triacontyl (C30) modified silica nanoparticles (NPs) into the polyacrylonitrile monolithic matrix through thermally induced phase separation. With efficient mass transfer and sorption capacity, C30 NP-PMC exhibited outstanding performance for the extraction of carotenoids and fat-soluble vitamins (FSVs) from human serum samples, superior to commercial C18 cartridges as well as liquid-liquid extraction (LLE) method. Under optimal conditions, the proposed µ-SPE method coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) achieved satisfactory limits of detection (LODs) (1.5-75.0 ng/mL) and good recoveries (85.0-106.5 %) with relative standard deviations (RSDs) of less than 12.1% by consuming lower sorbent (35.0 mg) and organic solvent (0.8 mL). Successful application of the developed method demonstrated the great potential of such monolithic sorbents for efficient isolation and preconcentration of trace analytes from blood samples.

Blu-Ray Discs as Universal Biochip Substrates: Lithography-Free Surface Activation and Assay Patterning.

Blu-ray discs (BDs) are advantageous in comparison with other optical discs (compact discs and digital versatile discs) in terms of not only their storage capacity but also the high-quality materials fabricated from. We have recently discovered that the "Hard Coat" film of Verbatim BDs is in fact a unique type of polymeric substrates that can be readily activated and adapted for biochip fabrications. Particularly, the Hard Coat film peeled from BDs is optically transparent without any fluorescence background, which can be activated by treating with a common base (1.0 M NaOH) at a slightly elevated temperature (55 °C). The surface density of reactive carboxylic acid groups generated, 6.6 ± 0.7 × 10-9 mol/cm2, is much higher than that on polycarbonate upon UV/ozone irradiation (4.8 ± 0.2 × 10-10 mol/cm2). There are no significant physical damages to the substrate morphology, and the aging effect is minimal. More importantly, the BD substrate can be patterned using either cut-out filter paper masks or microfluidic channel plates; both are lithography-free, bench-top methods that facilitate the device fabrication in a common laboratory setting. With classical biotin-streptavidin binding and DNA hybridization arrays as trial systems, we have also demonstrated this new type of biochip substrates for quantitative assay applications.

Co2+ detection, cell imaging, and temperature sensing based on excitation-independent green-fluorescent N-doped carbon dots.

Green-fluorescent N-doped carbon dots (N-CDs) have been successfully fabricated using hydrothermal treatment of tyrosine and urea. The N-CDs obtained showed excitation-independent emission, superior stability and strong photoluminescence with a quantum yield of ca. 9.8%. Based on these striking behaviors, the as-prepared N-CDs have been utilized in Co2+ detection and temperature sensing. Due to an inner filter effect, the N-CDs obtained were dramatically quenched by Co2+ with linear ranges of 0.1 µM-10 µM, 25 µM-275 µM and 300 µM-400 µM, and they had a detection limit of 0.15 µM. The use of the as-prepared N-CDs has been extended to visualize Co2+ fluctuations in living cells. Additionally, the N-CDs obtained have also been applied for use as a temperature sensor with a linear range of 25-80 °C.

Decreased levels of urinary free amino acids in children with autism spectrum disorder.

Autism spectrum disorder (ASD) is a range of neurodevelopmental problems without certain causes. Conventional diagnostic or screening tools for ASD rely on the observation of children's behavioral presentations. Novel methods are focused on the alterations of some important biochemical matters in ASD patients, which are applicable in the screening for ASD. This study investigated and compared amino acids in the first morning urine from age and sex matched ASD and non-ASD children using high performance liquid chromatography. Significantly lower urinary free methionine, phenylalanine, valine, tryptophan, and leucine plus isoleucine were observed in ASD children. The effects of using urinary free amino acids (UFAAs) singly or conjointly to classify participants into ASD or control group were analyzed and compared. ROC curves on these UFAAs singly in classification performed the sensitivity of 0.593-0.889 and the specificity of 0.704-0.963. Binary-logistic regression analysis of these UFAAs obtained a final regression model comprised of urinary free valine and tryptophan. The ROC curve established by the linear combination of the two amino acids achieved a sensitivity of 0.926 and a specificity of 0.889, which showed superiority to single UFAA and comparability to existing diagnostic or screening tools. It was suggested that the multivariate model based on UFAAs was possibly applicable in screening for children at higher risk of ASD.

Detection of ß-agonists in pork tissue with novel electrospun nanofibers-based solid-phase extraction followed ultra-high performance liquid chromatography/tandem mass spectrometry.

A selective analytical method based on packed-fiber solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry (PFSPE-UPLC-MS/MS) has been developed for determination of six ß-agonists (clorprenaline, bambuterol, clenbuterol, brombuterol, mabuterol, and penbuterol) in pork tissue. Polystyrene-polymeric crown ether (PS-PCE) composite nanofibers were fabricated by electrospinning and utilized to prepare the homemade extraction columns. With optimal conditions, all analytes were separated very well and the blank pork did not disturb the determination, and the linearity is good in a range of 5.0µg/kg-25.0µg/kg. The recoveries were 79.3-110.1%. RSDs for intra-day were in the range of 1.5-10.5% and RSDs for inter-day were 4.7-11.8%. Above all, only 5mg of sorbent and 200µL of elution solvent were favorable to directly extract all analytes in a complex matrix. The method is simple and cost-effective, and has the potential to be applied to quantitatively analyze the concentrations of polar species in food samples containing complex matrix.

Increased Cortisol and Cortisone Levels in Overweight Children.

BACKGROUND It has been unclear whether relatively high cortisol and cortisone levels are related to overweight in childhood, parental body mass index (BMI), and family dietary habits. The aim of this study was to compare cortisol and cortisone levels in urine and saliva from overweight and normal children, as well as correlations between children's BMI, parental BMI and family dietary behavior questionnaire score (QS). MATERIAL AND METHODS We analyzed the data from 52 overweight children and 53 age- and sex-matched normal-weight children aged 4-5 years. The concentrations of salivary cortisol (SF), salivary cortisone (SE), urinary cortisol (UF) and urinary cortisone (UE) were measured using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The family dietary behavior QS was answered by the parent mainly responsible for the family diet. RESULTS Average cortisol and cortisone levels were significantly higher in overweight children. There was no significant difference in the ratio of cortisol to cortisone (Rcc) and the marker of 11b-hydroxysteroid dehydrogenase type 2 (11ß-HSD2) activities. The results displayed correlations among cortisol, cortisone, and Rcc. Positive correlations were weak-to-moderate between BMI and SF, SE, UF, and UE. There were correlations between BMI and maternal BMI (mBMI), and BMI was significantly associated with QS. CONCLUSIONS Our results suggest that cortisol and cortisone levels are associated with overweight in children, but the 11ß-HSD2 activities showed no significant differences. Unhealthy family diet was associated with higher BMI, UF, and UE, and families with maternal overweight or obesity had a higher prevalence of children's overweight or obesity.

Application of packed-fiber solid-phase extraction coupled with GC-MS for the determination of short-chain fatty acids in children's urine.

BACKGROUND: Autism spectrum disorder (ASD) is a complex disorder involving interactions between genetic, epigenetic and environmental factors. Gastrointestinal (GI) disorders are prevalent in the cohort of children with ASD and they have been recognized as a comorbid condition recently. It is of value to monitor GI issues in individuals, and to help further characterize factors that may contribute to GI disorders (in individuals with and without ASD). Due to the biological relevance of short-chain fatty acids (SCFAs) to GI disorders, it is important to develop a rapid and selective detection method capable of identifying and quantifying SCFAs in complex biological samples. Because of low concentration and hydrophilicity of SCFAs, the pretreatment of sample becomes the key step to detection method. We erected and verified a packed-fiber solid-phase extraction (PFSPE) based on Polypyrrole (PPY) nanofibers coupled with gas chromatography-mass spectrometry (GC-MS) to determine SCFAs in urine. The proposed method was applied to detect SCFAs in urine from children with and without ASD, and the results between the 2 groups was compared. METHODS: PFSPE method was utilized for the direct pretreatment of SCFAs in urine from children. The SCFAs extracted on nanofibers was subsequently eluted with hydrochloric acid ethanol solution and detected by GC-MS. RESULTS: Intraday and interday assay CVs were ≤10%, and the recoveries was 82.6%-110.5%. Limit of detection (LOD) and limit of quantification (LOQ) were 0.25-2.67ng/ml and 0.85-8.97ng/ml, respectively. The level of SCFAs in urine from children with ASD were significantly higher than that from control group. CONCLUSION: The proposed method improves the simplification of sample treatment and displays sufficient analytical sensitivity and selectivity. The assay offers a potential to monitor the SCFAs in urine in clinical and experimental investigation of ASD.

Packed-Nanofiber solid phase extraction coupled with gas chromatography-mass spectrometry for the determination of phthalate esters in urines from children.

In this paper, we developed a rapid and safe method based on packed-fiber solid-phase extraction (PFSPE) system coupled with gas chromatography-mass spectrometry for the determination of four phthalate esters (PAEs), diethyl-o-phthalate (DEP), dibutyl-o-phthalate (DBP), di (2-ethylhexyl) phathalate (DEHP), di-n-octyl phthalate (DNOP), in urine samples. The PAEs in urine samples (500µL) were rapidly cleaned up from urines using polystyrene (PS) nanofibers packed micro-columns fitted on a PFSPE pretreatment device, which can process up to 12 samples simultaneously in 5min. Under optimum conditions, satisfied recovery and relative standard deviation values (RSDs) were in the range of 80.4-111.7% and 1.5-10.9%, respectively. The limits of detection (LOD) and the limits of quantification (LOQ) were ranged from 0.1 to 0.5ngmL-1 and 0.5-2ngmL-1, respectively. The well controlled matrix effect was also evaluated by comparing the signal response of the pure PAEs standards dissolved in methanol with the signal response of PAEs in the urine matrix. This new method was successfully applied to determine four PAEs in urine samples of overweight and normal-weight children, and an association between phthalates in urines and obesity was observed. Thus, the method seems to be a useful tool for monitoring of the level of urinary phthalate esters and also to support an evidence for further reasearch of obesity.

Comparison of Adsorption/Desorption of Volatile Organic Compounds (VOCs) on Electrospun Nanofibers with Tenax TA for Potential Application in Sampling.

The objective of this study was to compare the adsorption/desorption of target compounds on homemade electrospun nanofibers, polystyrene (PS) nanofibers, acrylic resin (AR) nanofibers and PS-AR composite nanofibers with Tenax TA. Ten volatile organic compounds (VOCs) were analyzed by preconcentration onto different sorbents followed by desorption (thermal and solvent orderly) and analysis by capillary gas chromatography. In comparison to Tenax TA, the electrospun nanofibers displayed a significant advantage in desorption efficiency and adsorption selectivity. Stability studies were conducted as a comparative experiment between PS-AR nanofibers and Tenax TA using toluene as the model compound. No stability problems were observed upon storage of toluene on both PS-AR nanofibers and Tenax TA over 60 hours period when maintained in an ultra-freezer (-80°C). The nanofibers provided slightly better stability for the adsorbed analytes than Tenax TA under other storage conditions. In addition, the nanofibers also provided slightly better precision than Tenax TA. The quantitative adsorption of PS-AR nanofibers exhibited a good linearity, as evidenced by the 0.988-0.999 range of regression coefficients (R). These results suggest that for VOCs sampling the electrospun nanofibers can be a potential ideal adsorbent.