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16 pages, 8003 KiB  
Article
Characterization of Cell Wall Compositions of Sodium Azide-Induced Brittle Mutant Lines in IR64 Variety and Its Potential Application
by Anuchart Sawasdee, Tsung-Han Tsai, Yi-Hsin Chang, Jeevan Kumar Shrestha, Meng-Chun Lin, Hsin-I Chiang and Chang-Sheng Wang
Plants 2024, 13(23), 3303; https://doi.org/10.3390/plants13233303 (registering DOI) - 25 Nov 2024
Viewed by 76
Abstract
The rice brittle culm is a cell wall composition changed mutant suitable for studying mechanical strength in rice. However, a thorough investigation of brittle culm has been limited due to the lack of diverse brittle mutants on similar genetic backgrounds in cell walls. [...] Read more.
The rice brittle culm is a cell wall composition changed mutant suitable for studying mechanical strength in rice. However, a thorough investigation of brittle culm has been limited due to the lack of diverse brittle mutants on similar genetic backgrounds in cell walls. In this study, we obtained 45 various brittle mutant lines (BMLs) from the IR64 mutant pool induced by sodium azide mutagenesis using the finger-bending method and texture profile analysis. The first scoring method was established to differentiate the levels of brittleness in rice tissues. The variation of cell wall compositions of BMLs showed that the brittleness in rice primarily correlated with cellulose content supported by high correlation coefficients (R = −0.78) and principal component analysis (PCA = 81.7%). As demonstrated using PCA, lower correlation with brittleness, hemicellulose, lignin, and silica were identified as minor contributors to the overall balance of cell wall compositions and brittleness. The analysis of hydrolysis and feeding indexes highlighted the importance of diversities of brittleness and cell wall compositions of BMLs and their potential applications in ruminant animals and making bioenergy. These results contributed to the comprehension of brittleness and mechanical strength in rice and also extended the applications of rice straw. Full article
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<p>The breaking force of a fresh flag leaf of 45 BMLs and IR64 at the maturity stage. Breaking force (N/mm) was the highest force required to break the sample when using the texture profile analyzer (TPA) divided by its leaf width. The error bar is SD obtained by three repetitions (<span class="html-italic">n</span> = 3).</p>
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<p>Diverse phenotypes of the BMLs from the IR64 mutant pool. (<b>A</b>) Pigmentation diversity in different tissues. (<b>B</b>) Diversity of leaf character. (<b>C</b>) Diversity of leaf green intensity by IRRI’s leaf color chart. (<b>D</b>) Diversity of grain characters (Bar = 1 cm).</p>
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<p>Correlation coefficients of phenotypes of BMLs. Larger numerical values and sizes indicate a stronger correlation. LL, leaf length; LW, leaf width; TH, time to heading date; SL, stem length; PN, panicle number; TM, time to maturity; PL, panicle length; GL, grain length; GW, grain width; GR, grain L/W ratio; PF, percentage of fertility; BF, breaking force. The interpretation of coefficient intervals: 0–0.19 (very low), 0.2–0.39 (low), 0.4–0.59 (middle), 0.6–0.79 (strong), and 0.8–1.0 (very strong). The asterisk indicates a significance (* = <span class="html-italic">p</span> &lt; 0.05; ** = <span class="html-italic">p</span> &lt; 0.01; *** = <span class="html-italic">p</span> &lt; 0.001).</p>
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<p>Correlation coefficient and principal component analysis of the cell wall compositions, breaking force, and brittleness score. (<b>A</b>) Correlation between the cell wall compositions: cellulose, hemicellulose, lignin, silica, brittleness score, and the breaking force of the flag leaf of brittle culm mutant lines was illustrated. Larger numerical values and sizes indicate a stronger correlation. The interpretation of coefficient intervals: 0–0.19 (very low), 0.2–0.39 (low), 0.4–0.59 (middle), 0.6–0.79 (strong), and 0.8–1.0 (very strong). The asterisk indicates a significance (** = <span class="html-italic">p</span> &lt; 0.01; *** = <span class="html-italic">p</span> &lt; 0.001). (<b>B</b>) Principal component analysis (PCA) biplot of BMLs on the phenotypic variables (arrows). The first two (PC1 + PC2) components accounted for 81.7% of the variance.</p>
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<p>The practice of BMLs for rice farming machinery. (<b>A</b>) Bar chart showing the average percentage of leaf damage in each brittleness score group after the Megi typhoon in 2016. The red arrow pointed to the damaged leaves. (<b>B</b>) Seedling of the brittle mutant line (AZ1805) was transplanted using a transplanting machine. (<b>C</b>) The grain of the brittle mutant line was harvested using a combiner. (<b>D</b>) The degradation of stubble of the brittle mutant line (<b>Left</b>) was faster than the wild type (<b>Right</b>).</p>
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<p>The hydrolysis means the wild type (IR64, score 0) and BMLs (score 5) within 24 h of incubation. * = significant difference by t-test (<span class="html-italic">p</span>-value &lt; 0.05).</p>
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18 pages, 4661 KiB  
Article
Pilot Study on a Liquid Mineral Foliar Fertilizer Mixed with Herbicides for Maize Protection and Nutrition
by Camelia Hodoșan, Lucica Nistor, Paula Poşan, Sorin Iulius Bărbuică, Daniela Ianiţchi, Gabriela Luţă and Lizica Szilagyi
Agriculture 2024, 14(12), 2129; https://doi.org/10.3390/agriculture14122129 - 24 Nov 2024
Viewed by 380
Abstract
The purpose of this study was to develop a complex composition of a foliar liquid mineral fertilizer containing NPK macroelements and microelements including Fe, Mg, B, S, Zn, Cu, Mo, Ni, V, and Cr. This complex fertilizer aims to support the optimal development [...] Read more.
The purpose of this study was to develop a complex composition of a foliar liquid mineral fertilizer containing NPK macroelements and microelements including Fe, Mg, B, S, Zn, Cu, Mo, Ni, V, and Cr. This complex fertilizer aims to support the optimal development and maturation of maize crops, thereby enhancing both the quality and quantity of production. In our study, an original recipe was established for a complex composition of foliar liquid mineral fertilizer, and a technological process was developed in order to obtain the recipe at the laboratory level. The designed fertilizer was a complex mixture of fertilizers with herbicides with multiple purposes, which can be used in different pedo-climatic areas and which present, at the same time, low toxicity and minimal ecological impact. A wide-spectrum mixture DICOPUR TOP containing 2,4-D acid and Dicamba was chosen as a systemic herbicide which is absorbed by plants both in the root system and also on the leaves. For conditioning the complex mixture of fertilizers with herbicides, different types of polyvinyl alcohol with different degrees of hydrolysis were used. The liquid fertilizer mixture with DICOPUR TOP was applied over two years (2021 and 2022) to the Felix maize hybrid, demonstrating significant positive effects on grain yield while effectively controlling both dicotyledonous and monocotyledonous weeds. Full article
(This article belongs to the Section Crop Protection, Diseases, Pests and Weeds)
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<p>Diagram of the laboratory installation used to make the complex composition of fertilizers (1—stand; 2—clamp; 3—gas bulb; 4—tripod; 5—balloon; 6—thermometer; 7—agitator; 8—refrigerant).</p>
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<p>Structural formulas of: (<b>a</b>) 2,4-D acid; (<b>b</b>) Dicamba.</p>
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<p>Temperatures (°C) recorded at the Moara Domneasca weather station, agricultural year 2020–2021.</p>
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<p>Precipitation (mm) recorded at the Moara Domneasca weather station, agricultural year 2020–2021.</p>
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<p>Temperatures (°C) recorded at the Moara Domneasca weather station, agricultural year 2021–2022.</p>
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<p>Precipitation (mm) recorded at the Moara Domneasca weather station, agricultural year 2021–2022.</p>
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<p><sup>1</sup>H-NMR spectrum of 2,4-D acid.</p>
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<p><sup>1</sup>H-NMR spectrum of Dicamba.</p>
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<p>The technological flow of manufacturing liquid foliar fertilizer.</p>
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<p>The new liquid foliar mineral fertilizer.</p>
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18 pages, 2935 KiB  
Article
Valorisation of Deinking Paper Sludge for Fertiliser Purposes: New Perspective in Sustainable Agriculture
by Halyna Kominko, Katarzyna Gorazda, Katarzyna Łoś and Zbigniew Wzorek
Agronomy 2024, 14(12), 2788; https://doi.org/10.3390/agronomy14122788 (registering DOI) - 24 Nov 2024
Viewed by 335
Abstract
The growth of the global population, coupled with concomitant economic development, has resulted in the generation of a substantial quantity of waste. The transition of the European Union’s economy towards a closed-loop model is prompting a comprehensive search for waste management concepts across [...] Read more.
The growth of the global population, coupled with concomitant economic development, has resulted in the generation of a substantial quantity of waste. The transition of the European Union’s economy towards a closed-loop model is prompting a comprehensive search for waste management concepts across a range of industrial sectors. The objective of this study is to valorise deinking paper sludge, which has a high potential for soil formation due to its high organic matter content. To produce organic–mineral fertiliser, the deinking sludge was subjected to acid hydrolysis, then neutralised with KOH solution and enriched with poultry litter ash. The final products were characterised in terms of their nutrient and heavy metal content. The bioavailability of phosphorus, along with the forms in which it occurs in fertilisers, was determined through the implementation of a five-step fractionation procedure. Furthermore, an eight-week incubation period was conducted to assess the fertilisers’ performance in soil. Soil samples were tested on a weekly basis for pH, water-soluble and bioavailable phosphorus content using the spectroscopic method after previous extraction in water and Bray’s solution, and catalase activity using the titrimetric method. The resulting fertilisers were found to meet the requirements for organo-mineral fertilisers and were categorised as PK-type fertilisers with a total nutrient content of 24.6–39.3%. Fractionation studies demonstrated that the fertilisers contained 20–30% of the total potentially bioavailable phosphorus. Furthermore, the long-term release of phosphorus from the fertilisers was confirmed through incubation studies. Additionally, the fertilisers were observed to contribute to an increase in catalase activity in the soil. Full article
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<p>Diagram of fertiliser production process.</p>
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<p>Composition of fertilisers.</p>
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<p>Phosphorus fractionation results.</p>
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<p>Changes in soil pH values during incubation studies.</p>
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<p>Changes in organic carbon content during incubation studies.</p>
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<p>Changes in water-soluble phosphorus content in soil during incubation studies.</p>
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<p>Changes in soil available phosphorus content during incubation studies.</p>
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<p>Changes in catalase activity during incubation studies.</p>
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18 pages, 5428 KiB  
Article
C/Ni/N Nanocomposites Based on Hydrolysis Lignin: Synthesis, Study of Structural and Magnetic Properties
by Ihor Bordun, Dariusz Calus, Ewelina Szymczykiewicz, Myroslav Malovanyy, Nazar Nahurskyi, Anatoliy Borysiuk and Yuriy Kulyk
Nanomaterials 2024, 14(23), 1886; https://doi.org/10.3390/nano14231886 - 23 Nov 2024
Viewed by 536
Abstract
A two-step method for the synthesis of C/Ni/N nanocomposites based on hydrolysis lignin from wood chemical processing waste is proposed. These nanocomposites were found to have a well-developed porous structure with a wide pore size distribution. It was shown that doping hydrolysis lignin [...] Read more.
A two-step method for the synthesis of C/Ni/N nanocomposites based on hydrolysis lignin from wood chemical processing waste is proposed. These nanocomposites were found to have a well-developed porous structure with a wide pore size distribution. It was shown that doping hydrolysis lignin with urea-derived nitrogen leads to the appearance of ferromagnetic behavior in the carbon material. When nickel chloride was added during pyrolysis, the magnetic behavior of the C/Ni/N composite was provided by superparamagnetic Ni particles less than 30 nm in size and the magnetism of the carbon matrix. The addition of urea during the synthesis of the nanocomposite further promotes better integration of nickel into the carbon structure. According to the results of magnetic studies, the nickel content in the C/Ni/N nanocomposite was 19 wt.% compared to 15 wt.% in the C/Ni nanocomposite. The synthesized nanocomposite was demonstrated to have no residual magnetization, so its particles do not agglomerate after the external magnetic field is removed. Due to this property and the well-developed porous structure, C/Ni/N composites have the potential to be used as catalysts, active electrode materials for autonomous energy sources, and in environmental technologies as magnetically sensitive adsorbents. Full article
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<p>General scheme for the synthesis of nanocomposites C/Ni/N.</p>
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<p>SEM images and EDX-mapping of the chemical element distribution of C/Ni/N (<b>a</b>), C/Ni (<b>b</b>) and C/N (<b>c</b>) samples.</p>
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<p>SEM images and EDX-mapping of the chemical element distribution of C/Ni/N (<b>a</b>), C/Ni (<b>b</b>) and C/N (<b>c</b>) samples.</p>
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<p>X-ray diffraction patterns of the synthesized nanocomposites C/Ni/N (<b>a</b>), C/Ni (<b>b</b>), and C/N (<b>c</b>).</p>
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<p>SAXS spectra of synthesized nanocomposites C/Ni/N (<b>a</b>), C/Ni (<b>b</b>) and C/N (<b>c</b>) (points—experimental data, solid line—smoothed curve).</p>
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<p>SAXS curves plotted in Porod coordinates <span class="html-italic">s</span><sup>4</sup><span class="html-italic">·I(s) = f(s</span><sup>4</sup><span class="html-italic">)</span> for C/Ni (<b>a</b>) and C/N (<b>b</b>) samples.</p>
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<p>Volume distribution functions of effective pore diameters for C/Ni/N (<b>a</b>), C/Ni (<b>b</b>) and C/N (<b>c</b>) samples.</p>
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<p>Nitrogen adsorption/desorption isotherms for the C/Ni/N (<b>a</b>), C/Ni (<b>b</b>) and C/N (<b>c</b>) samples.</p>
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<p>Pore size distribution for C/Ni/N (<b>a</b>), C/Ni (<b>b</b>) and C/N (<b>c</b>) samples calculated by the BJH method.</p>
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<p>Distribution of pores by size for C/Ni/N (<b>a</b>), C/Ni (<b>b</b>), and C/N (<b>c</b>) samples calculated by the MP method.</p>
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<p>Remagnetization curve of C/Ni/N nanocomposite. The inset shows a larger scale graph.</p>
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<p>Magnetic moment hysteresis curve of the C/Ni nanocomposite. The inset shows a larger scale graph.</p>
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<p>Temperature dependence of the saturation specific magnetization for C/Ni/N (<b>a</b>), C/Ni (<b>b</b>) and C/N (<b>c</b>) samples.</p>
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<p>Temperature dependences of the saturation specific magnetization: 1 of C/Ni/N composite, 2, 3—model temperature dependences for Ni nanoparticles and nitrogen-containing carbon C/N, respectively.</p>
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15 pages, 2056 KiB  
Article
Using Poly(amidoamine) PAMAM-βCD Dendrimer for Controlled and Prolonged Delivery of Doxorubicin as Alternative System for Cancer Treatment
by Kendra Sorroza-Martínez, Ignacio González-Sánchez, Raúl Villamil-Ramos, Marco Cerbón, Jorge Antonio Guerrero-Álvarez, Cristina Coronel-Cruz, Ernesto Rivera and Israel González-Méndez
Pharmaceutics 2024, 16(12), 1509; https://doi.org/10.3390/pharmaceutics16121509 - 23 Nov 2024
Viewed by 296
Abstract
Background/Objectives: Doxorubicin (Dox) is an anticancer drug used in the treatment of a wide range of solid tumors; however, Dox causes systemic toxicity and irreversible cardiotoxicity. The design of a new nanosystem that allows for the control of Dox loading and delivery results [...] Read more.
Background/Objectives: Doxorubicin (Dox) is an anticancer drug used in the treatment of a wide range of solid tumors; however, Dox causes systemic toxicity and irreversible cardiotoxicity. The design of a new nanosystem that allows for the control of Dox loading and delivery results is a powerful tool to control Dox release only in cancer cells. For this reason, supramolecular self-assembly was performed between a poly(amidoamine) (PAMAM) dendrimer decorated with four β-cyclodextrin (βCD) units (PAMAM-βCD) and an adamantane–hydrazone–doxorubicin (Ad-h-Dox) prodrug. Methods: The formation of inclusion complexes (ICs) between the prodrug and all the βCD cavities present on the surface of the PAMAM-βCD dendrimer was followed by 1H-NMR titration and corroborated by 2D NOESY experiments. A full characterization of the supramolecular assembly was performed in the solid state by thermal analysis (DSC/TGA) and scanning electron microscopy (SEM) and in solution by the DOSY NMR technique in D2O. Furthermore, the Dox release profiles from the PAMAM-βCD/Ad-h-Dox assembly at different pH values was studied by comparing the efficiency against a native βCD/Ad-h-Dox IC. Additionally, in vitro cytotoxic activity assays were performed for the nanocarrier alone and the two supramolecular assemblies in different carcinogenic cell lines. Results: The PAMAM-βCD/Ad-h-Dox assembly was adequately characterized, and the cytotoxic activity results demonstrate that the nanocarrier alone and its hydrolysis product are innocuous compared to the PAMAM-βCD/Ad-h-Dox nanocarrier that showed cytotoxicity equivalent to free Dox in the tested cancer cell lines. The in vitro drug release assays for the PAMAM-βCD/Ad-h-Dox system showed an acidic pH-dependent behavior and a prolonged profile of up to more than 72 h. Conclusions: The design of PAMAM-βCD/Ad-h-Dox consists of a new controlled and prolonged Dox release system for potential use in cancer treatment. Full article
(This article belongs to the Special Issue Cyclodextrin-Based Gene and Drug Delivery Applications)
13 pages, 1305 KiB  
Article
Mechanical Properties and In Vitro Digestibility of Fermented Lentil and Quinoa Flour Food Prototypes for Older Adults
by Elena Gomez-Gomez, Joaquim Calvo-Lerma, Mónica González, Ana Heredia, Amparo Tárrega and Ana Andrés
Nutrients 2024, 16(23), 4006; https://doi.org/10.3390/nu16234006 (registering DOI) - 23 Nov 2024
Viewed by 335
Abstract
Background/Objectives: The increase in the older adult population worldwide and the need to switch to vegetal-origin protein consumption for environmental sustainability point to legumes and pseudocereals as alternative ingredients in new food formulations. This study aimed to assess the impact of food [...] Read more.
Background/Objectives: The increase in the older adult population worldwide and the need to switch to vegetal-origin protein consumption for environmental sustainability point to legumes and pseudocereals as alternative ingredients in new food formulations. This study aimed to assess the impact of food structure and fungal fermentation on the digestibility of new food prototypes made with quinoa and/or lentil flours addressed to older adults. Methods: Four gels and six breads were elaborated and subjected to mechanical analysis and simulated gastrointestinal in vitro digestion. Then, proteolysis, lipolysis, and amylolysis were analysed. Results: Gels made with fermented quinoa or lentil flours exhibited less hardness and required less force, suggesting better adequacy for mastication. In terms of digestibility, using fermented flours led to increased proteolysis and reduced starch hydrolysis. Conclusions: Our results support future studies in the field aimed at supplying older adults with adapted foods to satisfy their nutritional needs to prevent sarcopenia and other health issues. Full article
(This article belongs to the Section Carbohydrates)
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<p>Proteolysis extent (%) of gel-like and bread-like prototypes after gastric and intestinal in vitro digestion under older adult conditions. Different lowercase letters indicate statistically significant differences among prototypes (<span class="html-italic">p</span> &lt; 0.05) at the gastric stage. Different capital letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05) among prototypes at the end of digestion. Unfermented (U), Fermented (F).</p>
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<p>Lipolysis extent (%) of gel-like and bread-like prototypes at the end of in vitro digestion under older adult conditions. Different capital letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05) among prototypes. Unfermented (U), Fermented (F).</p>
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<p>Amylolysis extent (%) of gel-like and bread-like prototypes at the end of in vitro digestion under older adult conditions. Different capital letters indicate statistically significant differences (<span class="html-italic">p</span> &lt; 0.05) among prototypes. Unfermented (U), Fermented (F).</p>
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16 pages, 3173 KiB  
Article
Functional Analysis of Two Carboxylesterase Genes Involved in Beta-Cypermethrin and Phoxim Resistance in Plutella xylostella (L.)
by Ran Li, Liang Liang, Yujia Zhao, Junyi Zhang, Zhiyuan Hao, Haibo Zhao and Pei Liang
Agronomy 2024, 14(12), 2781; https://doi.org/10.3390/agronomy14122781 (registering DOI) - 23 Nov 2024
Viewed by 300
Abstract
Enhanced expression of carboxylesterase (CarE) genes is an important mechanism of insecticide resistance in pests. However, their roles in multi-insecticide resistance have rarely been reported. Herein, two CarE genes (PxαE6 and PxαE9) were identified; their relative expression levels in three multi-insecticide-resistant [...] Read more.
Enhanced expression of carboxylesterase (CarE) genes is an important mechanism of insecticide resistance in pests. However, their roles in multi-insecticide resistance have rarely been reported. Herein, two CarE genes (PxαE6 and PxαE9) were identified; their relative expression levels in three multi-insecticide-resistant populations of P. xylostella (HN, GD-2017 and GD-2019) were 2.69- to 15.32-fold higher than those in the sensitive population, and they were considerably overexpressed at the larval stage and in the midgut of the 4th instar. PxαE6 and PxαE9 knockdown increased the susceptibility of GD-2019 larvae to phoxim or/and beta-cypermethrin. The recombinant PxαE6 and PxαE9 expressed in Escherichia coli exhibited high hydrolysis activity towards α-NA. GC–MS and LC–MS/MS assays revealed that PxαE9 could metabolize beta-cypermethrin and phoxim with efficiency determinations of 51.6% and 21.1%, respectively, while PxαE6 could metabolize phoxim with an efficiency of 12.0%. Homology modelling, molecular docking and molecular-dynamics simulation analyses demonstrated that beta-cypermethrin or/and phoxim could fit well into the active pocket and stably bind to PxαE6 or PxαE9. These results show that PxαE6 and PxαE9 overexpression were involved in resistance to beta-cypermethrin or/and phoxim in multi-insecticide-resistant P. xylostella populations, a finding which sheds light on the molecular mechanisms of multi-insecticide resistance in insect pests. Full article
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<p>CarE-specific activity of third-instars of <span class="html-italic">Plutella xylostella</span> from SS, HN, GD-2017 and GD-2019 populations. Means with distinct lowercase letters are significantly different.</p>
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<p>Relative expression of <span class="html-italic">PxaE6</span> and <span class="html-italic">PxαE9</span> in four populations (<b>A</b>,<b>B</b>) and various developmental stages (<b>C</b>,<b>D</b>) and body parts/tissues (<b>E</b>,<b>F</b>) of <span class="html-italic">Plutella xylostella</span>. SS, susceptible population. Three field populations: HN, GD-2017 and GD-2019. L1–L4, first to fourth instars. MT, malpighian tubule. The results are depicted as the mean ± standard deviation (<span class="html-italic">n</span> = 3), with bars labeled by distinct lowercase letters indicating a statistically significant difference (<span class="html-italic">p</span> &lt; 0.05) according to a one-way ANOVA followed by Tukey’s post hoc test.</p>
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<p>Relative expression of <span class="html-italic">PxaE6</span> (<b>A</b>) and <span class="html-italic">PxαE9</span> (<b>C</b>) in the 3rd larvae with dsRNA of selected <span class="html-italic">PxαE9</span> or ds<span class="html-italic">EGFP</span>. Mortalities of ds<span class="html-italic">PxαE6</span>- (<b>B</b>) and ds<span class="html-italic">PxαE9</span>-injected (<b>D</b>) third instars of <span class="html-italic">P. xylostella</span> 48 h post treatment with LC<sub>50</sub>. CYP, beta-cypermethrin; CHL, chlorantraniliprole; PHO, phoxim; TEB, tebufenozide; MET: metaflumizone. The asterisk * denotes a significant distinction between the treatment and control groups (Student’s <span class="html-italic">t</span>-test; <span class="html-italic">p</span> &lt; 0.05). Lowercase letters indicating a statistically significant difference (<span class="html-italic">p</span> &lt; 0.05) according to a one-way ANOVA followed by Tukey’s post hoc test.</p>
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<p>Analysis of recombinant PxαE6 and PxαE9 by SDS-PAGE (<b>A</b>) and WB assay (<b>B</b>). The recombinant proteins were fractionated on 10% gels, and WB analysis was conducted using an anti-His tag antibody. Lanes 1, pColdII vector with 0.5 mM IPTG; M, protein ladder; Lanes 2, recombinant vector of PxαE6 with 0.5 mM IPTG; Lanes 3, purified proteins of PxαE6; Lanes 4, recombinant vector of PxαE9 with 0.5 mM IPTG; Lanes 5, purified proteins of PxαE9. WB: Western blot.</p>
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<p>The catalytic kinetic parameters of recombinant PxαE6 (<b>A</b>) and PxαE9 (<b>B</b>). <span class="html-italic">V</span><sub>max</sub>, maximum velocity; <span class="html-italic">K</span><sub>m</sub>, Michaelis–Menten constant. Values are presented as mean ± standard error (SE).</p>
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<p>Residues of phoxim after incubation with purified recombinant PxαE6 (<b>A</b>). Residues of beta-cypermethrin (<b>B</b>) and phoxim (<b>C</b>) after incubation with purified PxαE9. Heat-inactivated recombinant PxαE6 or PxαE9 (boiled PxαE6 or PxαE9) and blank controls (no proteins were added) were used as double controls. The data were presented as mean ± standard deviation (SD) with n = 3 replicates. Bars labeled with distinct lowercase letters indicated significant differences (<span class="html-italic">p</span> &lt; 0.05) based on one-way ANOVA followed by Tukey’s multiple comparison test.</p>
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<p>The overall structure (left) and binding model (right) of PxαE6 and PxaE9 relative to insecticides. (<b>A</b>) PxαE6 and phoxim. (<b>B</b>) PxαE9 and beta-cypermethrin. (<b>C</b>) PxαE9 and phoxim. Note: Beta-cypermethrin and phoxim are represented in green and cyan, respectively. Gray, H; blue, N; red, O; green, Cl; firebrick, Br; yellow, S; orange, P. Residues of catalytic triad (Ser-Glu-His) are presented with deep-blue slate lines. Oxyanion holes are presented with green lines, anion sites are blue-colored lines and acyl binding pockets are shown with orange lines. Other amino acids which can form hydrogen bonds with pesticides are shown with yellow lines. The hydrogen bonds are shown with red dotted lines.</p>
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<p>(<b>A</b>–<b>D</b>) The binding models of PxαE9 and (<span class="html-italic">S</span>)-(1<span class="html-italic">R</span>, 3<span class="html-italic">R</span>)-beta-cypermethrin, (<span class="html-italic">R</span>)-(1<span class="html-italic">S</span>, 3<span class="html-italic">S</span>) -beta-cypermethrin, (<span class="html-italic">S</span>)-(1<span class="html-italic">R</span>, 3<span class="html-italic">S</span>) -beta-cypermethrin and (<span class="html-italic">R</span>)-(1<span class="html-italic">S</span>, 3<span class="html-italic">R</span>)-beta-cypermethrin. Note: The beta-cypermethrin molecule is depicted by green lines. Residues of catalytic triad (Ser-Glu-His) are represented with deep-blue slate lines. Anion sites are depicted with blue lines, oxyanion holes are represented with green lines, and acyl binding pockets are represented by orange lines. The hydrogen bonds are illustrated with red dotted lines.</p>
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8 pages, 2827 KiB  
Communication
Coordination of O-Propyl-N-phenylthiocarbamate to HgI2 and the Crystallographic Characterization of an Anilinium Chloride Thiocarbamate Adduct
by Wafa Arar, Nuri Ekici, Michael Knorr, Isabelle Jourdain, Carsten Strohmann and Jan-Lukas Kirchhoff
Molbank 2024, 2024(4), M1923; https://doi.org/10.3390/M1923 - 22 Nov 2024
Viewed by 232
Abstract
In order to investigate the coordination chemistry of O-alkyl N-aryl thiocarbamate ligands, HgI2 was reacted with one equivalent of PrOC(=S)N(H)Ph L in toluene solution to afford the 1D polymeric title compound [{IHg(μ-I)}{κ1-PrOC(=S)N(H)Ph}]n CP1. The formation [...] Read more.
In order to investigate the coordination chemistry of O-alkyl N-aryl thiocarbamate ligands, HgI2 was reacted with one equivalent of PrOC(=S)N(H)Ph L in toluene solution to afford the 1D polymeric title compound [{IHg(μ-I)}{κ1-PrOC(=S)N(H)Ph}]n CP1. The formation of this iodide-bridged coordination polymer was ascertained by a single-crystal X-ray diffraction study performed at 100 K, as well as the formation of an adduct between anilinium chloride and L forming a supramolecular ribbon of composition [L(PhNH3)(Cl)]. The occurrence of anilinium chloride is due to the partial hydrolysis of L in the presence of HCl. Full article
(This article belongs to the Section Organic Synthesis and Biosynthesis)
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<p>View of a segment of the supramolecular ribbon of PrOC(=S)NHPh•PhNH<sub>3</sub>Cl running along the <span class="html-italic">b</span> axis. Selected bond lengths (Å) and angles (deg). S–C1 1.6697(16), O–C1 1.329(2), O–C8 1.457(2), N1–C1 1.348(2), N1–C2 1.418(2), N2–C11 1.4674(19), C6–C5 1.386(3); C1–O–C8 119.18(12), O–C8–C9 112.09(14), O–C1–S 125.73(12), O–C1–N1 112.85(14), N1–C1–S 121.41(13), C1–N1–C2 131.79(15), C3–C2–N1 125.38(15). N2–H2A···Cl<sup>1</sup> 159.3, N2–H2B···Cl 171.5; N2–H2C···Cl<sup>2</sup> 162.6, N1–H1···Cl<sup>1</sup> 168.3. Symmetry transformation is used to generate equivalent atoms: <sup>1</sup>1/2-<span class="html-italic">x</span>, −1/2+<span class="html-italic">y</span>, 1/2-<span class="html-italic">z</span>; <sup>2</sup>1/2-<span class="html-italic">x</span>, 1/2 + <span class="html-italic">y</span>, 1/2-<span class="html-italic">z</span>.</p>
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<p><sup>1</sup>H NMR spectra (400 MHz, CDCl<sub>3</sub>) of <b>L</b> at 298 and 323 K. The * denotes CHCl<sub>3</sub>.</p>
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<p><sup>13</sup>C{<sup>1</sup>H} NMR spectrum (100 MHz, CDCl<sub>3</sub>) of <b>L</b> at 298 K. The * denotes CDCl<sub>3</sub>.</p>
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<p>View of a segment of <b>CP1</b> running along the <span class="html-italic">c</span> axis. Selected bond lengths (Å) and angles (deg). Hg–I1 2.6829(3), Hg–I2 2.9073(3), Hg–I2<sup>1</sup> 2.8421(3), Hg–S 2.5438(9), S–C5 1.710(4), O–C5 1.307(4), O–C6 1.473(4), N–C5 1.333(4), N–C9 1.430(4), C3–C7 1.390(5); I2<sup>1</sup>–Hg1–I2 103.989(9), I1– Hg1– I2 106.923(9), I1–Hg1–2<sup>1</sup> 116.402(9), S1–Hg1–I2<sup>1</sup> 98.49(2), S1–Hg1–I2 102.18(2), S1–Hg1– I1 126.21(2), Hg1<sup>2–</sup> I2-Hg 94.509(9), C5–O1–C6 120.0(3), C5–N1–C9 131.7(3), O–C5–S 121.5(3), O–C5–N 115.1(3), N–C5–S 123.4(3), O–C6–C10 105.9(3). Symmetry transformation is used to generate equivalent atoms: <sup>1</sup>+<span class="html-italic">x</span>, 1/2-<span class="html-italic">y</span>, 1/2 <span class="html-italic">z</span>; <sup>2</sup>+<span class="html-italic">x</span>, 1/2-<span class="html-italic">y</span>, −1/2+<span class="html-italic">z</span>.</p>
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<p>OLEX-generated view of the unit cell of <b>CP1</b>, indicating several intramolecular interactions by dotted lines (O2<b>···</b>H3C3 2.819(4) Å).</p>
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<p>Examples of some <span class="html-italic">O</span>-alkyl <span class="html-italic">N</span>-aryl thiocarbamate complexes.</p>
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<p>Synthesis of <b>L</b> and <b>CP1</b>.</p>
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12 pages, 5392 KiB  
Article
The Use of a Trichoderma reesei Culture for the Hydrolysis of Wheat Straw to Obtain Bioethanol
by Maria Ciobanu, Carmen Otilia Rusănescu and Raluca Lucia Dinculoiu
Processes 2024, 12(12), 2625; https://doi.org/10.3390/pr12122625 - 22 Nov 2024
Viewed by 265
Abstract
To reduce environmental pollution, a renewable source of energy that we may utilize is bioethanol obtained from wheat straw. Wheat straw was ground to 40–50 mm in size and heat-treated with high-pressure steam to release lignocelluloses, making them accessible to enzymes during saccharification. [...] Read more.
To reduce environmental pollution, a renewable source of energy that we may utilize is bioethanol obtained from wheat straw. Wheat straw was ground to 40–50 mm in size and heat-treated with high-pressure steam to release lignocelluloses, making them accessible to enzymes during saccharification. Through mechanical pretreatment, a substrate was obtained, which contains toxic components in concentrations that do not diminish the performance of the enzymes in the enzymatic hydrolysis phase. Through the thermal pretreatment of wheat straw, its acidity was improved, influencing the amounts of glucose, xylose, and other components emitted. Following enzymatic hydrolysis, very small concentrations of sugars were released. In order to increase the efficiency of the transformation of sugars into ethanol during the fermentation process, a strain of yeast, Trichoderma reesei multiplied in the laboratory, was added, under the conditions of temperature—28 degrees and stirring—800 rpm. Trichoderma reesei penetrated the wheat straw substrate, facilitating the subsequent hydrolysis process. The improved biodegradation of the pretreated straws was highlighted by the electron microscopy analysis. Full article
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<p>The process of obtaining bioethanol from lignocellulosic biomass (adapted from [<a href="#B14-processes-12-02625" class="html-bibr">14</a>]).</p>
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<p>Map of straw supply localities.</p>
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<p>Checking the quality of straw bales.</p>
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<p>Knives for cutting wheat straw.</p>
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<p>Sectioned straw sample.</p>
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<p>Sample substrate.</p>
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<p>Hydrolysate obtained after enzymatic hydrolysis.</p>
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<p><span class="html-italic">Trichoderma reesei</span> multiplied in the laboratory.</p>
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<p><span class="html-italic">Trichoderma reesei</span> transferred into production.</p>
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<p><span class="html-italic">Trichoderma reesei</span> in the last fermentation reactor.</p>
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<p>Scanning electron microscope (SEM) images (×1.00 kx magnification) indicating the inaccessible and packed structure of untreated and biotreated wheat straw. (<b>a</b>) Untreated wheat straw; (<b>b</b>) biotreated wheat straw (adapted from [<a href="#B2-processes-12-02625" class="html-bibr">2</a>]).</p>
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13 pages, 1961 KiB  
Article
Maximizing Collagen Yield from Underutilized Lumpfish (Cyclopterus lumpus) Skins by Optimizing Pre-Cleaning and Extraction Methods
by Judith Maria Scheja, Jens Jakob Sigurðarson, Halldór Gunnar Ólafsson and Hjörleifur Einarsson
Mar. Drugs 2024, 22(12), 525; https://doi.org/10.3390/md22120525 - 22 Nov 2024
Viewed by 331
Abstract
Female lumpfish (Cyclopterus lumpus) are a primary target of commercial fishery for their roe, a substitute for caviar. The remaining carcasses are underutilized rest raw material. The pre-treatment and acid extraction conditions of collagen from lumpfish skins were optimized. Full factorial [...] Read more.
Female lumpfish (Cyclopterus lumpus) are a primary target of commercial fishery for their roe, a substitute for caviar. The remaining carcasses are underutilized rest raw material. The pre-treatment and acid extraction conditions of collagen from lumpfish skins were optimized. Full factorial design was used to optimize the alkali pre-treatment conditions with NaOH. The optimal conditions were X1 = 0.1 M (NaOH concentration), X2 = 6 h (NaOH treatment time), X3 = 4 °C (treatment temperature) and X4 = 1:5 (w/v, solid to liquid ratio). Optimized conditions for collagen extraction with acetic acid were investigated using a Box–Behnken design. The result suggested a concentration of 0.9 M acetic acid, treatment temperature of 21 °C, a treatment time of 36 h in a total of 2 volumes of acid. Combined optimized effects resulted in a collagen yield of 45% (DW/DW) with high purity (>90%) and a high hydroxyproline content (7.9%). A scale-up experiment (starting with 45 kg) showed that the yield was somewhat lower (18–25%). Enzyme hydrolysis of skin after acetic acid extraction added another 23% (DW/DW) to the yield and enzyme hydrolysis of precleaned skins resulted in 60% (DW/DW). Full article
(This article belongs to the Special Issue Fishery Discards, Processing Waste and Marine By-Products)
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<p>Total amount (g) of proteins removed (<b>a</b>) and amount (mg) of hydroxyproline removed (<b>b</b>) by NaOH pre-treatment of 30 g skin samples at different conditions.</p>
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<p>Collagen and hydroxyproline extraction yields (%) (DW/DW) of samples extracted at 21 °C with acetic acid at different concentrations, ratios (<span class="html-italic">w</span>/<span class="html-italic">v</span>) and extraction times. Hydroxyproline yield is shown as mean ± SD. The center point at 0.5 M/1:5/24 h of the Box–Behnken design was performed in triplicate and is shown as an average with a standard deviation of 4% for the collagen yield.</p>
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<p>SDS-PAGE patterns of lumpfish skin collagen extracted at 21 °C. Lane L: molecular weight marker, lane 1–7: samples extracted for 24 h.</p>
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<p>SDS-page patterns of lumpfish skin collagen from 1 kg extraction. Lane L: molecular weight marker, lane 1–5: samples extracted for 36 h. Gel sliced at black line.</p>
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<p>Mass flow of dry weight (DW g) and collagen (COL, %) during acetic acid (AA) extraction and enzyme digestion of lumpfish skin. 100% DW equals 15.4 g at start and COL % is the collagen DW/DW yield. Collagen purity (P) is calculated as HYP% × 12.6. Acid Soluble Collagen (ASC); Enzyme Soluble Collagen (ESC).</p>
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<p>Workflow for the extraction of Acid Soluble Collagen (ASC) and Enzyme Soluble Collagen (ESC) from pre-treated lumpfish skins.</p>
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15 pages, 1934 KiB  
Article
Implementation of Sensitive Method for Determination of Benzophenone and Camphor UV Filters in Human Urine
by Veronika Gomersall, Katerina Ciglova and Jana Pulkrabova
Toxics 2024, 12(12), 837; https://doi.org/10.3390/toxics12120837 - 21 Nov 2024
Viewed by 292
Abstract
The level of the human body’s burden of benzophenone and camphor ultraviolet (UV) filters can be estimated from their urinary levels. The present study describes the implementations and validation of the sensitive analytical method for the analysis of seven benzophenone and two camphor [...] Read more.
The level of the human body’s burden of benzophenone and camphor ultraviolet (UV) filters can be estimated from their urinary levels. The present study describes the implementations and validation of the sensitive analytical method for the analysis of seven benzophenone and two camphor UV filters in urine. Sample preparation includes overnight enzymatic hydrolysis and ethyl acetate extraction followed by purification by dispersive solid-phase extraction using a sorbent Z-Sep. For the analysis, ultra-high performance liquid chromatography coupled with tandem mass spectrometry was used. Validation was performed using a Standard Reference Material® 3673 and an artificially contaminated urine sample. Target analyte recoveries ranged from 79–113% with repeatability expressed as a relative standard deviation of 2–15%. The limits of quantification were between 0.001 and 0.100 ng/mL in urine. This method was subsequently applied to examine the urine samples collected from Czech women. The analytes benzophenone-1 and 4-hydroxy-benzophenone were the most common analytes present in 100% of the samples, whereas benzophenone-3 was quantified in only 90% of the urine samples. The other four determined benzophenone derivatives were quantified in ≤33% of the samples. The derivatives of camphor were not detected in any samples. This method could be applied in biomonitoring studies. Full article
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<p>The influence of desolvation temperature on analyte response. Note: The desolvation temperature was tested with a capillary voltage set at ±4500 V. The data were normalised to analyte response at 500 °C. The analyte response was calculated from the qualifications transition from a standard solution of 10 ng/mL of the target analytes in methanol injected six times. The error bars correspond to relative standard deviations.</p>
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<p>The influence of capillary voltage on analyte response. Note: The capillary voltage was tested with a desolvation temperature set at 500 °C. The data were normalised to analyte response at ±4500 V. The analyte response was calculated from the qualifications transition from a standard solution of 10 ng/mL of the target analytes in methanol injected six times. The error bars correspond to relative standard deviations.</p>
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<p>The influence of mobile phase on analyte response. Note: The data were normalised to analyte response with (A) water and (B) methanol. The analyte response was calculated from the qualifications transition from a standard solution of 10 ng/mL of the target analytes in methanol injected six times. The error bars correspond to relative standard deviations.</p>
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<p>Extracted-ion chromatogram (XIC) of standard mixture of target analytes at concentration 10 ng/mL in methanol (HSS T3 C18 (100 mm × 2.1 mm × 1.8 µm) from Waters (Milford, MA, USA)).</p>
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<p>Extracted-ion chromatogram (XIC) of standard mixture of target analytes at concentration 10 ng/mL in methanol (PFP Kinetex (100 mm × 2.1 mm × 1.7 µm) from Phenomenex (Torrance, CA, USA)).</p>
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<p>Influence of urine matrix on ionisation of analytes.</p>
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22 pages, 8110 KiB  
Article
Synthesis and Physiochemical Properties of Sulphated Tamarind (Tamarindus indica L.) Seed Polysaccharide
by Sabrina Ziliani, Anna Alekseeva, Carlo Antonini, Emiliano Esposito, Fabio Neggiani, Marco Sansò, Marco Guerrini and Sabrina Bertini
Molecules 2024, 29(23), 5510; https://doi.org/10.3390/molecules29235510 - 21 Nov 2024
Viewed by 302
Abstract
Tamarind seed polysaccharide (TSP) is a neutral water-soluble galactoxyloglucan isolated from the seed kernel of Tamarindus indica with average molecular weight (Mw) 600–800 kDa. The high viscosity of TSP slows solubilisation, and the absence of charged substituent hinders the formation of electrostatic interactions [...] Read more.
Tamarind seed polysaccharide (TSP) is a neutral water-soluble galactoxyloglucan isolated from the seed kernel of Tamarindus indica with average molecular weight (Mw) 600–800 kDa. The high viscosity of TSP slows solubilisation, and the absence of charged substituent hinders the formation of electrostatic interactions with biomolecules. TSP was sulphated in a one-step process using dimethylformamide as a solvent, and sulphur trioxide-pyridine complex as a sulphating reagent. Studies of chemical structure, molecular weight distribution and viscosity were conducted to characterise the synthesised products. The sulphation degree was established by conductimetric titration; the sulphate group distribution was studied by NMR spectroscopy and liquid chromatography-mass spectrometry, and sulphated TSP oligomers were obtained by enzymatic degradation with cellulase and/or xyloglucanase. Sulphated products showed higher solubility than TSP, Mws in the range of 700–1000 kDa, a sulphation degree of two to four per subunit and pseudoplastic behaviour. A preliminary study of mucoadhesion revealed the unexpected interaction of S-TSP with mucin, providing a route by which sulphated TSP interactions with biomolecules may be influenced. Full article
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<p>Chemical structure of tamarind seed polysaccharide (TSP) isolated from the seed kernel of <span class="html-italic">Tamarindus indica</span>. TSP is composed of a β-(1,4)-<span class="html-small-caps">d</span>-glucan backbone, with α-(1,6)-<span class="html-small-caps">d</span>-xylose branches, partially substituted with β-(1,2)-<span class="html-small-caps">d</span>-galactose. The coloured residues and abbreviations in bold correspond to the observed monosaccharide, while the linked monosaccharides are shown in parentheses. Glc—glucose; Xyl—xylose; Gal—galactose.</p>
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<p>FT-IR spectra of TSP in black, S-TSP_1 in dark blue, S-TSP_2 in blue and S-TSP_3 in light blue. The new bands assigned to S=O and C–O–S stretching vibrations are signed with arrows.</p>
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<p>Chromatographic profile (red—refractive index; black—low laser light scattering; green—right angle light scattering; blue—viscometer) of pristine TSP (<b>a</b>) and S-TSP_1 (<b>b</b>).</p>
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<p>Viscosity curves of TSP in black, S-TSP_1 in dark blue, S-TSP_2 in blue and S-TSP_3 in light blue at 10 mg/mL at 20 °C.</p>
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<p><sup>1</sup>H-<sup>13</sup>C HSQC superimposition of the anomeric region of TSP in black and hydrolysed TSP, with xyloglucanase in red. The superscript corresponds to the carbon number of the observed monosaccharide, which is in bold, while the monosaccharide linked is in the parentheses. NR—non-reducing end; Glc—glucose; Xyl—xylose; Gal—galactose.</p>
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<p><sup>1</sup>H-<sup>13</sup>C HSQC superimposition of TSP in black and hydrolysed TSP with xyloglucanase in red. The superscript corresponds to the carbon number of the observed monosaccharide, which is in bold style, while the monosaccharide linked is in the parentheses. * signals assigned to the arabinose residue. Glc—glucose; Xyl—xylose; Gal—galactose.</p>
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<p>HILIC/ESI-QTOF-MS chromatograms of TSP hydrolysed by cellulase on the top and TSP hydrolysed by xyloglucanase on the bottom. Hex—hexose (glucose or galactose, 162 Da), P—pentose (xylose, 132 Da); the numbers in subscript indicate the number of hexoses and pentoses within the detected oligosaccharide: ox indicates the oxidized minor components (−2 Da), most likely related to the C4-oxidized oligomers, as previously reported by Sun et al. [<a href="#B29-molecules-29-05510" class="html-bibr">29</a>].</p>
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<p>IPRP-HPLC/ESI-QTOF-MS chromatogram of S-TSP hydrolysed by cellulase and xyloglucanase. Hex—hexose (glucose or galactose, 162 Da), P—pentose, (xylose, 132 Da), S—sulphate (SO<sub>3</sub>-, 80 Da); the numbers in subscript indicate the number of hexoses and pentoses within the detected oligosaccharide. The most abundant oligomers Hex<sub>6</sub>P<sub>3</sub>S<sub>x</sub> and Hex<sub>5</sub>P<sub>3</sub>S<sub>x</sub> are underlined and in bold. <span>$</span>—oligomers with the intensity lower than 500 (the intensity of the highest peaks Hex<sub>6</sub>P<sub>3</sub>S<sub>1</sub>/Hex<sub>5</sub>P<sub>3</sub>S<sub>1</sub> and Hex<sub>6</sub>P<sub>3</sub>S<sub>2</sub>/Hex<sub>5</sub>P<sub>3</sub>S<sub>2</sub> are higher than 1 × 10<sup>4</sup>).</p>
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<p>LC-MS chromatogram (<b>a</b>) and MS spectra of the most abundant peaks co-eluted in the regions of mono (<b>b</b>), bi- (<b>c</b>), tri- (<b>d</b>), tetra- (<b>e</b>), penta- (<b>f</b>) and hexasulphated (<b>g</b>) oligomers. Because various oligomers with the same sulphation degree, including positional isomers, are co-eluted, the mass spectra were averaged for their retention time range: 13.9–17.6 min ((<b>b</b>), Hex<sub>x</sub>P<sub>y</sub>S<sub>1</sub>); 18.6–22.6 min ((<b>c</b>), Hex<sub>x</sub>P<sub>y</sub>S<sub>2</sub>); 24.6–27.7 min ((<b>d</b>), Hex<sub>x</sub>P<sub>y</sub>S<sub>3</sub>); 31.0–34.3 min ((<b>e</b>), Hex<sub>x</sub>P<sub>y</sub>S<sub>4</sub>); 36.4–38.0 min ((<b>f</b>), Hex<sub>x</sub>P<sub>y</sub>S<sub>5</sub>); 41.7 ± 0.5 min ((<b>g</b>), Hex<sub>x</sub>P<sub>y</sub>S<sub>6</sub>). Hex—hexose (glucose or galactose, 162 Da), P—pentose, (xylose, 132 Da), S—sulphate (SO<sub>3</sub><sup>−</sup>, 80 Da); DBA—dibutylamine (129 Da, adducts are indicated with blue arrow); the numbers in subscript indicate the number of hexoses and pentoses within the detected oligosaccharide. The <span class="html-italic">m</span>/<span class="html-italic">z</span> values and the corresponding ion forms are reported in <a href="#app1-molecules-29-05510" class="html-app">Table S3</a>.</p>
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<p><sup>1</sup>H-<sup>13</sup>C HSQC superimposition of TSP in black hydrolysed with cellulase and S-TSP_1 hydrolysed with xyloglucanase and cellulase in blue. Circled signals are related to sulphation. Galactose anomeric signals, α and β, are reported in the figure. The superscript corresponds to the carbon number of the observed monosaccharide, which is in bold, while the monosaccharide linked is in the parentheses. * signals assigned to the cellulose enzyme; Gal—galactose.</p>
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<p>Viscosity curves: (<b>a</b>) TSP (10 mg/mL) in black and TSP with mucin (2.5 <span class="html-italic">w</span>/<span class="html-italic">w</span>) in red; (<b>b</b>) S-TSP_1 (10 mg/mL) in blue and S-TSP_1 with mucin (2.5 <span class="html-italic">w</span>/<span class="html-italic">w</span>) in red.</p>
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18 pages, 9524 KiB  
Article
Synthesis, Characterization, and Application Prospects of Novel Soluble Polysilsesquioxane Bearing Glutarimide Side-Chain Groups
by Yuliya I. Bolgova, Artem I. Emel’yanov, Olga M. Trofimova, Anastasiya A. Ivanova, Alexander I. Albanov, Nadezhda P. Kuznetsova, Tatyana A. Semenova and Alexander S. Pozdnyakov
Polymers 2024, 16(23), 3235; https://doi.org/10.3390/polym16233235 - 21 Nov 2024
Viewed by 273
Abstract
The requirement for the development of advanced technologies is the need to create new functional thermostable soluble polysilsesquioxanes. Combining the potential of organosilicon chemistry and the chemistry of heterocyclic compounds is a promising direction for the formation of novel organosilicon polymer systems with [...] Read more.
The requirement for the development of advanced technologies is the need to create new functional thermostable soluble polysilsesquioxanes. Combining the potential of organosilicon chemistry and the chemistry of heterocyclic compounds is a promising direction for the formation of novel organosilicon polymer systems with new properties and new possibilities for their practical application. Using the classical method of hydrolysis and polycondensation of previously unknown trifunctional (trimethoxysilylpropyl)glutarimide in the presence or absence of an acid or base catalyst, a universal approach to the formation of new thermostable soluble polysilsesquioxanes with glutarimide side-chain groups is proposed, which forms the basis for the synthesis of polysilsesquioxane polymers with different functionality. The weight average molecular weight of silsesquioxanes, determined by gel permeation chromatography, is practically independent of the reaction conditions and is 10–12 kDa; at the same time, the molecular weight distribution remains low and amounts to 1.38–1.47. According to thermogravimetric analysis, the resulting polysiloxanes have high thermal stability up to 335 °C. By the dynamic light scattering method, it was established that in an aqueous solution, silsesquioxane macromolecules are in an associated state, forming supramolecular structures due to the intermolecular interaction of individual macromolecules. The average hydrodynamic diameter of the particles was 46 nm. X-ray diffraction analysis showed the amorphous nature of the polymer. Polymer film coatings based on synthesized silsesquioxanes are characterized by 98% transmission in the visible spectrum and resistance to ultraviolet radiation, which is promising for the creation of functional transparent film coatings. Full article
(This article belongs to the Special Issue Silicon-Based Polymers: From Synthesis to Applications)
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<p>Images of the 1-[3-(trimethoxysilyl)propyl]piperidine-2,6-dione (<b>a</b>) and 1-[3-(silsesquioxanyl)propyl]piperidine-2,6-dione <b>2a</b> (<b>b</b>).</p>
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<p>FTIR spectra of 1-[3-(trimethoxysilyl)propyl]piperidine-2,6-dione (<b>1</b>) and 1-[3-(silsesquioxanyl)propyl]piperidine-2,6-dione (<b>2a</b>–<b>c</b>).</p>
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<p><sup>1</sup>H NMR spectra of 1-[3-(trimethoxysilyl)propyl]piperidine-2,6-dione (down) and 1-[3-(silsesquioxanyl)propyl]piperidine-2,6-dione (<b>2a</b>) (up).</p>
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<p><sup>13</sup>C NMR spectra of 1-[3-(trimethoxysilyl)propyl]piperidine-2,6-dione (down) and 1-[3-(silsesquioxanyl)propyl]piperidine-2,6-dione <b>2a</b> (up).</p>
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<p>GPC curves of silsesquioxanes <b>2a</b>–<b>c</b>: a—pH 7, b—pH 3, and c—pH 10.</p>
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<p>Unit structures for siloxanes and silsesquioxanes.</p>
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<p><sup>29</sup>Si NMR spectra of 1-[3-(silsesquioxanyl)propyl]piperidine-2,6-dione (<b>2a</b>–<b>c</b>).</p>
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<p>XRD pattern of polysilsesquioxane <b>2a</b>.</p>
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<p>Distribution of effective diameters of scattering particles of PSQ-GI <b>2a</b>: (<b>a</b>) in aqueous salt solution and (<b>b</b>) in water.</p>
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<p>1-[3-(Silsesquioxanyl)propyl]piperidine-2,6-dione <b>2a</b>: (<b>a</b>) in aqueous salt solution (unassociated state) and (<b>b</b>) in water (associated state).</p>
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<p>TGA (black line) and DSC (blue line) curves of PSQ-GI <b>2a</b> (under air, 5 °C/min).</p>
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<p>Mass spectra of PSQ-GI <b>2a</b> under air.</p>
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<p>Photograph of a water droplet: (<b>a</b>) deposited on the surface of PSQ-GI polymer film coating on silicate glass and (<b>b</b>) deposited on untreated silicate glass.</p>
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<p>UV-Vis spectrum and photographs (inset) of a polymer-coated glass substrate (<b>a</b>) and an uncoated glass substrate (<b>b</b>).</p>
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<p>The synthetic route of 1-[3-(trimethoxysilyl)propyl]piperidine-2,6-dione <b>1</b>.</p>
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<p>The synthetic route of 1-[3-(silsesquioxanyl)propyl]piperidine-2,6-dione.</p>
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12 pages, 1266 KiB  
Article
The Role of Unsaturated Fatty Acid-Rich Dairy Products in Adipocyte Metabolism
by Manuela Machado, Eduardo M. Costa, Sara Silva, Ana Maria Gomes and Manuela Pintado
Molecules 2024, 29(23), 5502; https://doi.org/10.3390/molecules29235502 - 21 Nov 2024
Viewed by 279
Abstract
This study investigated the fatty acid profile, permeability, and metabolic effects of a functional yogurt enriched with pomegranate oil, focusing on its impact on lipid metabolism and inflammatory responses. The yogurt’s fatty acid composition was primarily composed of long-chain polyunsaturated fatty acids (54.37%), [...] Read more.
This study investigated the fatty acid profile, permeability, and metabolic effects of a functional yogurt enriched with pomegranate oil, focusing on its impact on lipid metabolism and inflammatory responses. The yogurt’s fatty acid composition was primarily composed of long-chain polyunsaturated fatty acids (54.37%), followed by saturated (29.34%) and monounsaturated fatty acids (16.36%). During in vitro digestion, a shift in fatty acid profile was observed, with a decrease in polyunsaturated and saturated fatty acids and a slight increase in monounsaturated fatty acids due to hydrolysis. This study further analyzed fatty acid permeability across Caco-2/HT29-MTX monolayers and 3T3-L1 cell uptake, revealing higher permeability for saturated fatty acids than unsaturated ones. In 3T3-L1 cells, permeated fatty acids induced higher lipolysis and increased adiponectin secretion without affecting leptin levels. Cytokine analysis indicated a decrease in pro-inflammatory markers, such as MCP-1, and a significant increase in anti-inflammatory cytokines like IL-10, suggesting potential benefits in reducing obesity-related inflammation. These results underscore the role of functional yogurts enriched with polyunsaturated fatty acids as promising agents for modulating lipid metabolism and inflammatory responses. Full article
(This article belongs to the Special Issue Bioorganic Chemistry in Europe)
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<p>Effect of in vitro digestion on fatty acid quantitative profile. C14, myristic acid; C16, palmitic acid; C18, stearic acid; C18:1 <span class="html-italic">c</span>9, oleic acid; C18:1 <span class="html-italic">c</span>11, <span class="html-italic">cis</span>-vaccenic acid; C18: 2 <span class="html-italic">c</span>9<span class="html-italic">c</span>12, linoleic acid; C20:1, <span class="html-italic">cis</span>-gondoic acid; C18:3 <span class="html-italic">c</span>9<span class="html-italic">c</span>12<span class="html-italic">c</span>15, linolenic acid; C18:3 <span class="html-italic">c</span>9<span class="html-italic">t</span>11<span class="html-italic">c</span>13, punicic acid; C18:3 <span class="html-italic">c</span>9<span class="html-italic">t</span>11<span class="html-italic">t</span>13, α-eleostearic acid; C18:3 <span class="html-italic">t</span>9<span class="html-italic">t</span>11<span class="html-italic">c</span>13, catalpic acid; C18:3 <span class="html-italic">t</span>9<span class="html-italic">t</span>11<span class="html-italic">t</span>13, β-eleostearic acid; ns means no significant differences, and * means significant differences as determined by a one-way ANOVA test (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Pomegranate oil yogurt cytotoxicity toward the target cell lines. CT is the negative control (40% <span class="html-italic">v/v</span> DMSO). The dotted line represents the 30% cytotoxicity limit as defined by ISO 10993–5 [<a href="#B18-molecules-29-05502" class="html-bibr">18</a>]. **** means significant differences as determined by a one-way ANOVA test (<span class="html-italic">p</span> &lt; 0.001).</p>
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<p>Effect of permeated pre-digested yogurt on lipolysis (<b>A</b>) and adipokine (adiponectin (<b>B</b>) and Leptin (<b>C</b>)) secretion in 3T3-L1 cells after 24 h of exposure. POY—pomegranate oil yogurt; ns means no significant differences, and * and **** means significant differences as determined by a one-way ANOVA test (<span class="html-italic">p</span> &lt; 0.05 and <span class="html-italic">p</span> &lt; 0.001).</p>
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<p>Cytokine production on the 3T3-L1 complex co-culture model basolateral side by the Caco-2/HT29-MTX membrane. POY—pomegranate oil yogurt; ns means no significant differences, and *, ** and *** means significant differences as determined by a one-way ANOVA test (<span class="html-italic">p</span> &lt; 0.05, <span class="html-italic">p</span> &lt; 0.01 and <span class="html-italic">p</span> &lt; 0.001).</p>
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27 pages, 1840 KiB  
Review
Nutritional Composition and Functional Properties of A. platensis-Derived Peptides: A Green and Sustainable Protein-Rich Supplement
by Nabila Begum, Fei Qi, Fang Yang, Qudrat Ullah Khan, Faizan, Qiang Fu, Jie Li, Xiu Wang, Xiaoxiao Wang, Jun Wang, Riwang Li, Dahai Liu and Wenqing Zhang
Processes 2024, 12(11), 2608; https://doi.org/10.3390/pr12112608 - 20 Nov 2024
Viewed by 381
Abstract
Among cyanobacterium, Arthrospira platensis (A. platensis) is a rich source of diverse bioactive compounds due to its high protein, essential amino acid, vitamin, and mineral content. A. platensis is one of the most abundant sources of protein (50–70%). In the food industry, [...] Read more.
Among cyanobacterium, Arthrospira platensis (A. platensis) is a rich source of diverse bioactive compounds due to its high protein, essential amino acid, vitamin, and mineral content. A. platensis is one of the most abundant sources of protein (50–70%). In the food industry, A. platensis is being used as an ingredient for the development of food flavor, taste, and nutritional composition. Several in vitro and in vivo studies have revealed the potential use of A. platensis in the prevention and treatment of various metabolic diseases. Recently, extensive research has focused on the production and bioactivity of the A. platensis-derived bioactive peptides. A series of steps were used for the production of bioactive peptides including hydrolysis, ultrafiltration, and chromatographic techniques, coupled with an advanced detector. A. platensis peptides showed health benefits such as anti-hypertension, anti-diabetes, anti-microbial, antioxidant, anti-obesity, and anti-cancer activities. This review aims to present the main nutritional composition of A. platensis, the processes of purification, and the identification of bioactive peptides, and the potential health benefits such as antihypertensive, antidiabetic, anti-cancer, anti-obesity, antioxidant, and anti-microbial activities associated with the consumption of A. platensis-derived peptides are discussed. The originality of this review over the old review is that our review comprehensively studies the macro- and micronutrient composition and listed bioactive peptides to date, which can play an important role in the treatment of various diseases. Moreover, this review provides information related the research gaps of the various technologies that should be used for the development of the peptide as a pharmaceutical and functional food. Full article
(This article belongs to the Section Food Process Engineering)
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<p>Nutritional composition (macro- and micronutrients) of <span class="html-italic">A. platensis</span>.</p>
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<p>Systematic overview of the extraction, isolation, purification, and identification of bioactive peptides from <span class="html-italic">A. platensis</span>.</p>
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<p>Potential health benefits and mechanism of action associated with <span class="html-italic">A. platensis</span>-derived peptides.</p>
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