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1.
J Chromatogr A ; 1736: 465321, 2024 Aug 30.
Artículo en Inglés | MEDLINE | ID: mdl-39255651

RESUMEN

Oligonucleotides (ONs) are acquiring clinical relevance and their demand is expected to grow. However, the ON production capacity is currently limited by high manufacturing costs. Since the purification of the target ON sequence from molecularly similar variants represents a major bottleneck, this work presents a resource-effective strategy for the optimization of their preparative reversed-phase chromatographic purification. First, a model based on the equilibrium-dispersive theory was introduced to describe the chromatographic operation. Considering a deoxyribose nucleic acid with 20 nucleobases as case study, a genetic algorithm was developed to efficiently determine the adsorption isotherm and mass transfer parameters for the target ON and impurities. After the estimation of these parameters, a strategy for the in-silico optimization of the operation was established. The product collection window, gradient duration, and resin loading were considered as process variables and their influence on yield and productivity was investigated after setting a purity specification of 99.0%. The optimal process parameters identified through this analysis were experimentally verified, confirming the reliability of the model, calibrated with only 5 experimental runs. In addition, this optimal setpoint was exploited to design the multicolumn countercurrent solvent gradient purification (MCSGP) of this ON mixture, which allowed to boost the yield of the process and to work at cyclic steady state, while respecting the purity constraint. This study confirmed the potential of this in-silico optimization strategy in both improving the performance of the traditional single-column operations and in the rapid development of multicolumn processes.

2.
Anal Chim Acta ; 1326: 343139, 2024 Oct 16.
Artículo en Inglés | MEDLINE | ID: mdl-39260917

RESUMEN

BACKGROUND: Several oxylipins including hydroxy- and epoxy-polyunsaturated fatty acids act as lipid mediators. In biological samples they can be present as non-esterified form, but the major part occurs esterified in phospholipids (PL) or other lipids. Esterified oxylipins are quantified indirectly after alkaline hydrolysis as non-esterified oxylipins. However, in this indirect analysis the information in which lipid class oxylipins are bound is lost. In this work, an untargeted liquid chromatography high-resolution mass spectrometry (LC-HRMS) method for the direct analysis of PL bearing oxylipins was developed. RESULTS: Optimized reversed-phase LC separation achieved a sufficient separation of isobaric and isomeric PL from different lipid classes bearing oxylipin positional isomers. Individual PL species bearing oxylipins were identified based on retention time, precursor ion and characteristic product ions. The bound oxylipin could be characterized based on product ions resulting from the α-cleavage occurring at the hydroxy/epoxy group. PL sn-1/sn-2 isomers were identified based on the neutral loss of the fatty acyl in the sn-2 position. A total of 422 individual oxPL species from 7 different lipid classes i.e., PI, PS, PC, PE, PC-P, PC-O, and PE-P were detected in human serum and cells. This method enabled to determine in which PL class supplemented oxylipins are incorporated in HEK293 cells: 20:4;15OH, 20:4;14Ep, and 20:5;14Ep were mostly bound to PI. 20:4;8Ep and 20:5;8Ep were esterified to PC and PE while other oxylipins were mainly found in PC. SIGNIFICANCE: The developed LC-HRMS method enables the comprehensive detection as well as the semi-quantification of isobaric and isomeric PL species bearing oxylipins. With this method, we show that the position of the oxidation has a great impact and directs the incorporation of oxylipins into the different PL classes in human cells.


Asunto(s)
Espectrometría de Masas , Oxilipinas , Fosfolípidos , Oxilipinas/análisis , Oxilipinas/química , Humanos , Fosfolípidos/análisis , Fosfolípidos/química , Espectrometría de Masas/métodos , Cromatografía Liquida/métodos , Isomerismo
3.
Molecules ; 29(17)2024 Sep 08.
Artículo en Inglés | MEDLINE | ID: mdl-39275104

RESUMEN

Fungal infections are among the most common diseases of crop plants. Various species of the Fusarium spp. are naturally prevalent and globally cause the qualitative and quantitative losses of farming commodities, mainly cereals, fruits, and vegetables. In addition, Fusarium spp. can synthesize toxic secondary metabolites-mycotoxins under high temperature and humidity conditions. Among the strategies against Fusarium spp. incidence and mycotoxins biosynthesis, the application of biological control, specifically natural plant extracts, has proved to be one of the solutions as an alternative to chemical treatments. Notably, rowanberries taken from Sorbus aucuparia are a rich source of phytochemicals, such as vitamins, carotenoids, flavonoids, and phenolic acids, as well as minerals, including iron, potassium, and magnesium, making them promising candidates for biological control strategies. The study aimed to investigate the effect of rowanberry extracts obtained by supercritical fluid extraction (SFE) under different conditions on the growth of Fusarium (F. culmorum and F. proliferatum) and mycotoxin biosynthesis. The results showed that various extracts had different effects on Fusarium growth as well as ergosterol content and mycotoxin biosynthesis. These findings suggest that rowanberry extracts obtained by the SFE method could be a natural alternative to synthetic fungicides for eradicating Fusarium pathogens in crops, particularly cereal grains. However, more research is necessary to evaluate their efficacy against other Fusarium species and in vivo applications.


Asunto(s)
Fusarium , Micotoxinas , Extractos Vegetales , Sorbus , Fusarium/efectos de los fármacos , Fusarium/metabolismo , Fusarium/crecimiento & desarrollo , Micotoxinas/biosíntesis , Extractos Vegetales/farmacología , Extractos Vegetales/química , Sorbus/química , Ergosterol/biosíntesis
4.
Heliyon ; 10(17): e37255, 2024 Sep 15.
Artículo en Inglés | MEDLINE | ID: mdl-39296210

RESUMEN

Renewable lignocellulosic biomass is a favorable energy resource since its co-pyrolysis with hydrogen-rich plastics can produce high-yield and high-quality biofuel. In contrast to earlier co-pyrolysis research that concentrated on increasing product yield, this study comprehends the synergistic effects of two distinct feedstocks that were not considered earlier. This work focuses on co-pyrolyzing wheat straw (WS) with non-reusable polyethylene terephthalate (PET) for the production of pyrolysis oil. WS and PET were blended in different ratios (100/0, 80/20, 60/40, 40/60, 20/80, and 0/100), and pyrolysis experiments were conducted in a fixed-bed reactor under different temperatures to assess their synergistic effect on oil yield. Synergy rates of up to 7.78 % were achieved on yield for the blends of plastic and biomass at a temperature of 500 °C. In comparison to individual biomass or plastics, co-pyrolyzing PET-biomass blends demonstrated good process interaction and promoted the yields of value-added products. The heating value of the pyrolysis oils was in the range of 16.45-28.64 MJ/kg, which depends on the amount of plastic present in the feedstock. The physical analysis of the oils shows that they can be used for heat production by direct combustion in boilers or furnaces. The correlation between WS and PET was validated with the aid of Fourier transform infrared spectroscopy (FT-IR) and gas chromatography-mass spectrometry (GC-MS) analysis. The GC-MS result demonstrated the presence of different compounds such as O-H compounds, esters, carbonyl group elements, acids, hydrocarbons, aromatics, and nitrogenated compounds in the pyrolysis oil, which differed based on the proportions of PET in the feedstock. The increased hydrocarbon and reduced oxygen percentages in the pyrolysis oil were implicitly caused by enhanced hydrocarbon pool mechanisms, in which the breakdown of PET may be supplied as a hydrogen donor. Overall, waste lignocellulosic biomass and plastics can be used to produce biofuels, which helps reduce the amount of solid waste that ends up in landfills. This study also revealed that future research should be focused on the reaction mechanisms of WS and PET co-pyrolysis in order to examine the synergistic interactions.

5.
Urolithiasis ; 52(1): 125, 2024 Sep 06.
Artículo en Inglés | MEDLINE | ID: mdl-39237676

RESUMEN

Laser lithotripsy mechanisms can cause the chemical decomposition of stone components and the emergence of different end products. However, the potentially toxic end products formed during thulium fiber laser (TFL) lithotripsy of cystine stones have not been sufficiently investigated. The aim of our in vitro study is to analyze the chemical content of the gas products formed during the fragmentation of cystine stone with TFL. Human renal calculi consisting of 100% pure cystine, calcium oxalate monohydrate, or uric acid were fragmented separately with TFL in experimental setups and observed for gas release. After the lithotripsy, only the cystine stones showed gas formation. Gas chromatography-mass spectrometry was used to analyze the gas qualitatively, and scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX) and X-ray diffraction was used to examine the dried cystine stone fragments. Fragmentation of the cystine stones released free cystine, sulfur, hydrogen sulfide, and carbon disulfide gas. The SEM-EDX and X-ray diffraction analyses revealed that the free cystine in the dried fragments contained 43.1% oxygen, 28.7% sulfur, 16.1% nitrogen, and 12.1% carbon atoms according to atomic weight. The detection of potentially toxic gases after lithotripsy of cystine stones with TFL indicates a risk of in vivo production. Awareness needs to be increased among healthcare professionals to prevent potential inhalation and systemic toxicity for patients and operating room personnel during TFL lithotripsy of cystine stones.


Asunto(s)
Oxalato de Calcio , Cistina , Litotripsia por Láser , Microscopía Electrónica de Rastreo , Tulio , Ácido Úrico , Cistina/análisis , Cistina/química , Humanos , Oxalato de Calcio/análisis , Oxalato de Calcio/química , Litotripsia por Láser/métodos , Ácido Úrico/análisis , Tulio/química , Cálculos Renales/química , Cálculos Renales/terapia , Gases/análisis , Cromatografía de Gases y Espectrometría de Masas , Difracción de Rayos X
6.
Sci Rep ; 14(1): 19107, 2024 08 17.
Artículo en Inglés | MEDLINE | ID: mdl-39154140

RESUMEN

Nekemias grossedentata (N. grossedentata) is a medicinal and edible plant. The young leaves and tender stems are specifically utilized to manufacture vine tea, which is traditionally employed in the treatment of conditions such as the common cold fever, sore throat, jaundice hepatitis, and other ailments. The morphologically of N. grossedentata similar to Nekemias cantoniensis (N. cantoniensis) and Nekemias megalophylla (N. megalophylla), which lead to a chaotic market supply. Numerious studies have confirmed that chloroplast genomes and chromatography play important role in plant classification. Here, the whole chloroplast (cp) genomes of the three Nekemias species were sequenced in Illumina sequencing platform. Meanwhile, their chromatographic fingerprints have constructed using high-performance liquid chromatography (HPLC). The annotation results demonstrated that the three chloroplast genomes were typical quadripartite structures, with lengths of 162,147 bp (N. grossedentata), 161,981 bp (N. megalophylla), and 162,500 bp (N. cantoniensis), respectively. A total of 89 (N. grossedentata) /86 (N. megalophylla and N. cantoniensis) protein-coding genes, 37 tRNA gene and 8 rRNA genes were annotated. The IR/SC boundary regions were relatively conserved across the three species, although three regions (rps19-rpl2, rpl32-trnL-UAG, ccsA-ndhD) exhibited nucleotide diversity values (Pi) of variable sites higher than 1%. Phylogenetic analysis indicated that N. grossedentata had a closer genetic relationship with N. megalophylla than that of N. cantoniensis. Moreover, the chromatographic fingerprints revealed that the main functional components and genetic relatedness of three species were highly similar with their morphological results. In conclusion, N. grossedentata and N. megalophylla can be consider as the origin plants of vine tea. This study provides appropriate information for species identification, phylogeny, quality assessment of three medicinal plants of the genus Nekemias and will contribute to the standardization of vine tea raw materials.


Asunto(s)
Genoma del Cloroplasto , Filogenia , Té/genética
7.
J Chromatogr A ; 1732: 465218, 2024 Sep 13.
Artículo en Inglés | MEDLINE | ID: mdl-39106663

RESUMEN

We describe a non-chromatographic, ligand-free platform for the efficient purification of recombinant human lactoferrin (LF). The platform consists of a [metal:chelator] complex precipitate in the presence of osmotically active polyethylene glycol 6000 (PEG-6000). Purification is achieved in three stages. Following formation of the complex, LF is captured under neutral conditions by the aggregated complexes (Step I), a washing step follows (Step II) and then, (Step III) LF is extracted in pure form with 100 mM tribasic Na citrate buffer (pH 7). Of the four complexes investigated, [bathophenanthroline (batho)3:Fe2+] was determined to be the most efficient. LF is recovered with high yield (∼90%, by densitometry) and purity (≥97%, by SDS polyacrylamide gel electrophoresis (SDS-PAGE)) from an artificial contamination background comprising E. coli lysate proteins. Purified LF is demonstrated to be monomeric by dynamic light scattering (DLS); to preserve its native secondary structure by circular dichroism (CD) spectroscopy; and, as apo-LF, to efficiently inhibit bacterial growth. Process yield is not affected by a 45-fold increase in LF concentration from 0.2 to 9 mg/mL. We provide evidence that protein capture relies on [cation:π] interactions between the lysine and arginine residues of LF with the fully aromatic [(batho)3:Fe2+] complexes. The use of [metal:chelator] complex aggregates is demonstrated to provide an economical and efficient avenue for LF purification.


Asunto(s)
Lactoferrina , Humanos , Lactoferrina/aislamiento & purificación , Lactoferrina/química , Fenantrolinas/química , Proteínas Recombinantes/aislamiento & purificación , Proteínas Recombinantes/química , Electroforesis en Gel de Poliacrilamida , Dicroismo Circular , Polietilenglicoles/química , Hierro/química
8.
J Sep Sci ; 47(15): e2400415, 2024 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-39118576

RESUMEN

Porous cage materials with certain dimensions, sizes, shapes, and functions have been regarded as promising materials for sample preparation, chromatographic separation, and detection process. In contrast to infinite frameworks such as metal-organic frameworks or covalent organic frameworks, porous cage materials are constructed from discrete molecules containing at least one internal cavity. The well-defined cavities in porous cage materials provide opportunities for non-covalent interactions. These interactions can be programmed into the ligand design or supramolecular cage constructing using the cages as building blocks, offering various host-guest recognition with great selectivity. In this review, we desire to elucidate the fundamental principles governing the design and fabrication of porous cage materials with well-defined cavities, good solvent processability, and modifiable groups, the applications of these porous cage materials in sample preparation, chromatographic separation, and detection were discussed. The recent advantages of porous cage materials for the analysis process were summarized. We state the potential of these materials and provide an outlook for further application strategies. We expect that this review can inspire interest in the porous cage materials research area for analysis.

9.
Se Pu ; 42(8): 805-811, 2024 Aug.
Artículo en Chino | MEDLINE | ID: mdl-39086250

RESUMEN

Tobacco flavor, an important tobacco additive, is an essential raw material in cigarette production that can effectively improve the quality of tobacco products, add aroma and taste, and increase the suction flavor. The quality consistency of tobacco flavors affects the quality stability of branded cigarettes. Therefore, the quality control of tobacco flavors is a major concern for cigarette and flavor manufacturers. Physical and chemical indices, odor similarity, and sensory efficacy are employed to evaluate the quality of tobacco flavors, and the analysis of chemical components in tobacco flavors is usually conducted using gas chromatography (GC) and high performance liquid chromatography (HPLC). However, because the composition of tobacco flavors is complex, their quality cannot be fully reflected using a single component or combination of components. Therefore, establishing an objective analytical method for the quality control of tobacco flavors is of extreme importance. Chromatographic fingerprint analysis is routinely used for the discriminative analysis of tobacco flavors. Chromatographic fingerprints refer to the general characteristics of the concentration profiles of different chemical compounds. In the daily procurement process, fingerprints established by GC and HPLC are effective for the evaluation and identification of tobacco flavors. However, given continuous improvements in aroma-imitation technology, some flavors with high similarity cannot be directly distinguished using existing methods. In this study, a method for the determination of organic acids and inorganic anions in tobacco flavors based on ion chromatography (IC) was developed to ensure the quality consistency of tobacco flavors. A 1.0 g sample of tobacco flavors and 10 mL of deionized water were mixed and vibrated for 30 min. The aqueous sample solution was passed through a 0.45 µm membrane filter and RP pretreatment column in succession to eliminate interferences and then subjected to IC. Standard solutions containing nine organic acids and seven inorganic anions were used to identify the anions in the tobacco flavors, and satisfactory reproducibility was obtained. The relative standard deviations (RSDs) for retention times and peak areas were <0.71% and <6.02%, respectively. The chromatographic fingerprints of four types of tobacco flavors (samples A-D) from five different batches were obtained. Nine tobacco flavor samples from different manufacturers (samples AY1-AY3, BY1-BY2, CY1-CY2, DY1-DY2) were also analyzed to obtain their chromatographic fingerprints. Hierarchical cluster and similarity analyses were used to evaluate the quality of tobacco flavors from different manufacturers. Hierarchical clustering refers to the process of subdividing a group of samples into clusters that exhibit a high degree of intracluster similarity and intercluster dissimilarity. The dendrograms obtained using SPSS 12.0 indicated good quality consistency among the samples in different batches. Samples AY3, BY2, CY2, and DY1 clustered with the batches of standard tobacco flavors. Therefore, hierarchical cluster analysis can effectively distinguish the quality of products from different manufacturers. The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine (version 2.0) was used to evaluate the similarity between the standard tobacco flavors and products from different manufacturers. Among the samples analyzed, samples AY3, BY2, CY2, and DY1 showed the highest similarity values (>97.7%), which was consistent with the results of the hierarchical cluster analysis. This finding indicates that IC combined with chromatographic fingerprint analysis could accurately determine the quality of tobacco flavors. GC combined with ultrasonic-assisted liquid-liquid extraction was also used to analyze the tobacco flavors and verify the accuracy of the proposed method. Compared with GC coupled with ultrasonic-assisted liquid-liquid extraction, IC demonstrated more significant quality differences among certain tobacco flavors.


Asunto(s)
Nicotiana , Control de Calidad , Nicotiana/química , Aromatizantes/análisis , Productos de Tabaco/análisis , Cromatografía Líquida de Alta Presión/métodos , Cromatografía de Gases/métodos , Cromatografía por Intercambio Iónico/métodos
10.
J Chromatogr A ; 1734: 465279, 2024 Oct 11.
Artículo en Inglés | MEDLINE | ID: mdl-39197362

RESUMEN

Cordyceps genus is entomopathogenic mushrooms that have traditionally been used in ethnomedicine in Asian countries. Nucleosides (Ns), nucleotide(Nt), Nucleobases (Nb) and their analogues play a critically physiological role and have a great potential in drug development, such as pentostatin and cordycepin (COR). Due to their significance bioactivity, several Nt/Ns were used as markers for quality evaluation for medicinal Cordyceps, including adenosine, inosine, guanosine, uridine and COR. Among them, COR is the most considerable adenosine analogue, exhibiting significant therapeutic potential and has many intracellular targets. Nt/Ns contains polar compounds and the phosphate groups of Nt deprotonate and carry negative charges with a broad range of pH values. Recent years, various advanced methods of extraction and separation, and nanomaterials have been developed to extract, isolate and determine these molecules, such as ultrasound-assisted extraction (UAE), Supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE) for the extraction, the solid phase extraction (SPE) methods (microextraction SPE (SPME), magnetic SPE (MSPE), and unique SPE materials based on the boronate affinity for the separation, and chromatography methods employing ultraviolet (UV), fluorescence, MS detection and electrospray ionization (ESI), along with matrix-assisted laser desorption/ ionization (MALDI) for the determination. COR derived from adenosine and its structure is very similar to that of 2'-deoxyadenosine (2'-dA) and adenosine, resulting in an incorrect identification, which will influence its therapeutic effects. Therefore, this review primarily focused on the characteristics of Nt/Ns, the advanced methods, strategies, nanomaterials for extracting and determining Nt/Ns (COR in particular) in Cordyceps spp, as well as the methods for distinguishing COR from its structure analogs.


Asunto(s)
Cordyceps , Nucleósidos , Nucleótidos , Cordyceps/química , Nucleósidos/análisis , Nucleósidos/aislamiento & purificación , Nucleótidos/análisis , Nucleótidos/aislamiento & purificación , Nucleótidos/química , Desoxiadenosinas
11.
Talanta ; 280: 126768, 2024 Dec 01.
Artículo en Inglés | MEDLINE | ID: mdl-39197312

RESUMEN

In response to the challenges associated with the chromatographic separation of polar compounds, this study aims to devise a solution by introducing a novel stationary phase. Hydrogels, characterized by a three-dimensional network structure, have aroused wide attention owing to its functional designability, multiple interaction sites and good adhesion, etc. In this work, an adhesive hydrogel functionalized silica stationary phase (Sil@PVA/TA) was synthesized using physical coating technique. Due to the co-existence of hydroxyl and benzene ring in the hydrogel structure, the obtained composites materials exhibited excellent separation performance for various of compounds and excellent column efficiency up to 71385.6 plates/m for thymidine. Furthermore, the hydrogel functionalized silica demonstrated superior selectivity to bare silica, diol-column and NH2-column for the separation of various of polar molecules, including, nucleosides/bases, alkaloids, organic acids, antibiotics and amino acids. Notably, for alkaloids, which frequently encounter peak tailing issues, Sil@PVA/TA demonstrated superior peak shape compared with C18 column. In short, this study successfully synthesized a hydrogel functionalized silica stationary phase, offering a novel method for the separation and analysis of polar compounds.

12.
Phytochem Anal ; 2024 Aug 05.
Artículo en Inglés | MEDLINE | ID: mdl-39103224

RESUMEN

INTRODUCTION: Schisandrae Chinensis Fructus (SCF), a traditional Chinese medicine, has been used in treating virtual injury and strain since ancient times. The Chinese Pharmacopoeia reveals that SCF includes raw (RSCF) and vinegar-processed (VSCF) decoction pieces. OBJECTIVE: This study developed an effective method combining the electronic eye (e-eye), electronic tongue (e-tongue), and chemometrics to discriminate RSCF and VSCF from the perspective of chemical composition, color, and taste. MATERIAL AND METHODS: First, RSCF were collected and processed into VSCF, and their color parameters, e-tongue sensory properties, high-performance liquid chromatography (HPLC) and ultra-HPLC (UPLC) characteristic fingerprints, and nominal ingredients were determined. Multivariate statistical analyses, including principal component, linear discriminant, similarity, and partial least squares discriminant analyses, were conducted. RESULTS: HPLC and UPLC fingerprints were established, demonstrating a > 0.900 similarity. The content determination indicated increased schisantherin A, schisantherin B, and schisandrin A contents in VSCF. The e-eye data demonstrated a > 1.5 total color difference before and after processing ΔE*ab, indicating the significantly changed sample color and appearance before and after processing. The e-tongue technology was used to quantitatively characterize the taste of RSCF and VSCF. The t-test revealed significantly reduced sourness, aftertaste-bitter, and aftertaste-astringent values of SCF after vinegar processing. Principal component and partial least squares discriminant analyses indicated that e-eye and e-tongue realize the rapid RSCF and VSCF identification. CONCLUSION: The proposed comprehensive strategy of electronic eye and electronic tongue combined with chemometrics demonstrated satisfactory results with high efficiency, accuracy, and reliability. This can be developed into a novel and accurate method for discriminating RSCF and VSCF.

13.
J Chromatogr A ; 1732: 465227, 2024 Sep 13.
Artículo en Inglés | MEDLINE | ID: mdl-39116685

RESUMEN

Styrene-maleic acid (SMA) copolymer has received much attention for its excellent solubilization characteristics. In this work, SMA copolymer brush-based chromatographic stationary phases were exploited and developed for the first time. First, SMA copolymer brush was in situ grown on the surface of spherical silica via living/controlled reversible addition-fragmentation chain transfer (RAFT) polymerization method. Subsequently, as a proof-of-concept demonstration, the copolymer was esterified by diethylene glycol mono-2-ethylhexyl ether (DGME) and 2-(2-ethylhexyloxy) ethanol (EHOE), respectively. The obtained Sil-SMA-DGME and Sil-SMA-EHOE copolymer-brush chromatographic stationary phases were characterized by transmission electron microscopy, Fourier transform infrared spectrometer, X-ray photoelectron spectroscopy, and thermogravimetric analysis, respectively. The chromatographic retention mechanism indicated that both the two packed columns exhibited hydrophilic/reverse mixed-mode retention modes. The maximum column efficiency was up to 71,000 N/m. The chromatographic separation performance evaluation indicated that the novel kind of stationary phases had excellent separation capabilities for hydrophilic, hydrophobic compounds and phospholipid standards. In addition, by combination with mass spectrometry identification, the Sil-SMA-DGME column was further exploited for separation and identification of phospholipids in human lung cancer cells. Totally, 9 classes including 186 phospholipid species were successfully identified. The results demonstrated the promising application prospects of the novel kind of SMA copolymer-brush chromatographic stationary phases.


Asunto(s)
Maleatos , Dióxido de Silicio , Maleatos/química , Dióxido de Silicio/química , Humanos , Interacciones Hidrofóbicas e Hidrofílicas , Poliestirenos/química , Esterificación , Cromatografía Líquida de Alta Presión/métodos , Polímeros/química
14.
Sci Rep ; 14(1): 19942, 2024 08 27.
Artículo en Inglés | MEDLINE | ID: mdl-39198548

RESUMEN

Clay vessels have a wide variety of functions in social activities in the Hallstatt period. In addition to food storage and processing, they were used for ritual purposes and as funerary vessels. The paper presents the results of archaeological and chromatographic studies of 31 vases from two different Hallstatt culture sites in lower Silesia (Poland). The investigations included vessels fragments from the Domaslaw cemetery and from the Milejowice settlement. The chromatographic analyses focused on fatty acids and biomarkers and made it possible to identify the most likely sources of substances they came into contact with during use. The c-means and hierarchical cluster analyses showed that grave vessels differed from settlement ceramics. Thus, conclusions on the diverse vessel functions could be made.


Asunto(s)
Cementerios , Cerámica , Polonia , Cerámica/historia , Humanos , Arqueología , Historia Antigua , Ácidos Grasos/metabolismo
15.
Food Chem ; 461: 140782, 2024 Dec 15.
Artículo en Inglés | MEDLINE | ID: mdl-39151341

RESUMEN

The hibiscus calyx contains 0.3-2.4% total anthocyanins, and is a promising source for naturally red food colorants. In this study, commercially available hibiscus calyces were subjected to ethanolic-aqueous extraction and chromatographic enrichment with the XAD-7HP resin, to create scalable, high-anthocyanin and low-acidity natural food colorants. Anthocyanins, organic and phenolic acids were monitored after each step using UHPLC-DAD and UHPLC-QQQ/MS. 75.67% total anthocyanins were recovered from calyces after double extractions, and the content increased by 8.50-14.90 times after the column enrichment, reaching 14.51-31.90% (by dry weight) in the final product. Chromatographic fractionation was also shown to effectively increase the total phenolic acids by 11.01-16.22 times, and remove an average of 98.58% of the total organic acids. High intensity redness at pH 2.5-3.5 indicated that the final product may be a promising, versatile natural food and beverage colorant in low pH products.


Asunto(s)
Antocianinas , Colorantes de Alimentos , Hibiscus , Extractos Vegetales , Hibiscus/química , Antocianinas/química , Antocianinas/análisis , Colorantes de Alimentos/química , Colorantes de Alimentos/análisis , Colorantes de Alimentos/aislamiento & purificación , Cromatografía Líquida de Alta Presión , Extractos Vegetales/química , Flores/química
16.
J Chromatogr A ; 1733: 465249, 2024 Sep 27.
Artículo en Inglés | MEDLINE | ID: mdl-39178658

RESUMEN

Geometric isomers tend to have similar polarities and differ only in molecular shape. Vigorously developing new stationary phases to meet the requirements for the separation of isomers that have similar physicochemical properties is still an urgent topic in separation science. Poly (arylene ether)-based dendrimers are known for their multifunctional branched peripheral structures and high self-assembly properties. In this paper, two amphiphilic dendritic organic small molecule gelling agents based on poly (aryl ether), PAE-ANT and PAE-PA, were prepared and conjugated to the silica surface. SiO2@PAE-ANT and SiO2@PAE-PA were used as HPLC stationary phases for the separation of non-polar shape-restricted isomers. Both stationary phases have very high molecular shape selectivity for isomers such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), tocopherols and carotenoids. Separation of cis-trans geometric isomers such as diethylstilbestrol and polar compounds such as monosubstituted benzenes and anilines can also be achieved. These two columns offer more flexible selectivity and higher separation performance than commercial C18 and phenyl columns. There is a difference in molecular shape selectivity between the two stationary phases for the same analyte test probes. SiO2@PAE-ANT showed slightly better linear selectivity for non-polar shape-restricted isomers compared to SiO2@PAE-PA with Janus-type PAE-PA bonding phase. This separation behavior may be attributed to the ordered spatial structure formed by the gel factor on the surface of the stationary phase and the combined effect of multiple weak interaction centers (hydrophobic, hydrophilic, hydrogen bonding and π-π interactions). It was also possible to separate nucleoside and nucleobase strongly polar compounds well in the HILIC mode, suggesting that hydrophilic groups in PAE-ANT and PAE-PA are involved in the interactions, reflecting their amphiphilic nature. The results show that the ordered gelation of dendritic organic small molecule gelators on the SiO2 surface, along with multiple carbonyl-π, π-π and other interactions, play a crucial role in the separating shape-restricted isomers. The integrated and ordered functional groups serve as the primary driving force behind the exceptionally high molecular shape selectivity of SiO2@PAE-ANT and SiO2@PAE-PA phases. Alterations in the structure of dendritic organic small molecule gelators can impact both molecular orientation and recognition ability, while changes in the type of functional groups influences the separation mechanism of shape-restricted isomers.


Asunto(s)
Dendrímeros , Dióxido de Silicio , Dióxido de Silicio/química , Cromatografía Líquida de Alta Presión/métodos , Isomerismo , Dendrímeros/química , Hidrocarburos Policíclicos Aromáticos/química , Hidrocarburos Policíclicos Aromáticos/análisis , Hidrocarburos Policíclicos Aromáticos/aislamiento & purificación , Bifenilos Policlorados/química , Bifenilos Policlorados/análisis , Bifenilos Policlorados/aislamiento & purificación , Carotenoides/química , Carotenoides/análisis , Carotenoides/aislamiento & purificación , Tensoactivos/química
17.
J Chromatogr A ; 1731: 465180, 2024 Aug 30.
Artículo en Inglés | MEDLINE | ID: mdl-39053255

RESUMEN

Novel magnetic covalent organic frameworks (COFs) were prepared by one-pot synthetic strategy and employed as an efficient adsorbent for magnetic solid-phase extraction (MSPE) of naphthaleneacetic acid (NAA) in food samples. Depending on the predesigned the hydrogen bonding, π-π and hydrophobic interactions of magnetic COFs, the efficient and selective extraction process for NAA was achieved within 15 min. The magnetic COFs adsorbent combined with HPLC-UV was devoted to develop a novel quantitative method for NAA in complex food. The method afforded good coefficient in range of 0.002-10.0 µg mL-1 and low limit of detection was 0.0006 µg mL-1. And the newly established method afforded less adsorbent consumption, wider linearity and lower LODs than the reported analytical methods. Ultimately, the method was successfully applied to determine NAA in fresh pear, tomato and peach juice. The magnetic COFs based MSPE coupled with HPLC-UV method provided a simple, efficient and dependable alternative to monitor trace NAA in food samples.


Asunto(s)
Límite de Detección , Estructuras Metalorgánicas , Ácidos Naftalenoacéticos , Extracción en Fase Sólida , Extracción en Fase Sólida/métodos , Cromatografía Líquida de Alta Presión/métodos , Ácidos Naftalenoacéticos/análisis , Ácidos Naftalenoacéticos/química , Estructuras Metalorgánicas/química , Adsorción , Contaminación de Alimentos/análisis , Solanum lycopersicum/química , Jugos de Frutas y Vegetales/análisis
18.
Materials (Basel) ; 17(14)2024 Jul 18.
Artículo en Inglés | MEDLINE | ID: mdl-39063862

RESUMEN

Detecting temperature and concentration fields within engine combustors holds paramount significance in enhancing combustion efficiency and ensuring operational safety. Within the realm of engine combustors, the laminar absorption spectroscopy technique has garnered considerable attention. Particularly crucial is the optimization of the optical path configuration to enhance the efficacy of reconstruction. This study presents a flame parameter field reconstruction model founded on laminar absorption spectroscopy. Furthermore, an optimization approach for refining the optical path configuration is delineated. In addressing non-axisymmetric flames, the simulated annealing algorithm (SA) and Harris's Hawk algorithm (HHO) are employed to optimize the optical path layout across varying beam quantities. The findings underscore a marked reduction in imaging errors with the optimized optical path configuration compared to conventional setups, thereby elevating detection precision. Notably, the HHO algorithm demonstrates superior performance over the SA algorithm in terms of optimization outcomes and computational efficiency. Compared with the parallel optical path, the optimized optical path of the HHO algorithm reduces the temperature field error by 25.5% and the concentration field error by 26.5%.

19.
Molecules ; 29(14)2024 Jul 10.
Artículo en Inglés | MEDLINE | ID: mdl-39064851

RESUMEN

Pyrrolizidine alkaloids (PAs) are toxic compounds that occur naturally in certain plants, however, there are many secondary pathways causing PA contamination of other plants, including medicinal herbs and plant-based food products, which pose a risk of human intoxication. It is proven that chronic exposure to PAs causes serious adverse health consequences resulting from their cytotoxicity and genotoxicity. This review briefly presents PA occurrence, structures, chemistry, and toxicity, as well as a set of analytical methods. Recently developed sensitive electrochemical and chromatographic methods for the determination of PAs in honey, teas, herbs, and spices were summarized. The main strategies for improving the analytical efficiency of PA determination are related to the use of mass spectrometric (MS) detection; therefore, this review focuses on advances in MS-based methods. Raising awareness of the potential health risks associated with the presence of PAs in food and herbal medicines requires ongoing research in this area, including the development of sensitive methods for PA determination and rigorous legal regulations of PA intake from herbal products. The maximum levels of PAs in certain products are regulated by the European Commission; however, the precise knowledge about which products contain trace but significant amounts of these alkaloids is still insufficient.


Asunto(s)
Productos Biológicos , Alcaloides de Pirrolicidina , Alcaloides de Pirrolicidina/análisis , Humanos , Productos Biológicos/análisis , Productos Biológicos/química , Plantas Medicinales/química , Espectrometría de Masas/métodos , Contaminación de Alimentos/análisis , Toxinas Biológicas/análisis
20.
Plants (Basel) ; 13(14)2024 Jul 11.
Artículo en Inglés | MEDLINE | ID: mdl-39065442

RESUMEN

Phedimus aizoon has been utilized as a medicinal plant in Asia. However, the production of phytochemical-rich extracts from P. aizoon and the evaluation of their bioactivity are limited. Herein, phytochemical-rich extracts were prepared by ultrasound-assisted extraction of P. aizoon, with a high extraction yield of 16.56%. The extracts contained about 126 mg of phenolics and 31 mg of flavonoids per g of the extracts. The chromatographic analysis (GC-MS and HPLC analyses) identified 19 notable phytochemicals of the extracts from P. aizoon, including pentacosane, hexadecanoic acid, gallic acid, vanillic acid, and quercetin. The gallic acid content of the extracts was relatively high at 2.75 mg/g. The identified compounds are known to have various bioactivities, such as antioxidant, antibacterial, and antifungal activities. In fact, the prepared extracts exhibited antioxidant activity at 24-28% of that of ascorbic acid. In addition, it showed antibacterial activity against both Escherichia coli (Gram-negative bacteria) and Staphylococcus aureus (Gram-positive bacteria). This study highlights that P. aizoon deserves attention as a natural bioactive substance and emphasizes the need for applications of the extracts from P. aizoon.

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