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1.
Inflammopharmacology ; 32(2): 1333-1351, 2024 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-37994993

RESUMEN

Biocompatible anti-inflammatory lignin-capped Ag (LCAg) nanoparticles (NPs) were synthesized for the delivery of galloyl ß-sitosterol (Galloyl-BS). ß-Sitosterol (BS) is effective against inflammatory responses, like cancer-induced inflammations. BS was modified via gallic acid esterification to enhance its anti-inflammatory potential. LCAg NPs were synthesized by a green method and loaded with galloyl-BS. For comparison, pure BS was also loaded onto LCAg NPs in a separate assembly. The antioxidant potential of Galloyl-BS was greater (IC50 177 µM) than pure BS. Materials were characterized by FT-IR, SEM, XRD, and Zeta potential. Using UV-Vis spectroscopy, drug release experiments were performed by varying pH, time, concentration, and temperature. Maximum drug release was observed after 18 h at pH 6 and 40 °C. Galloyl-BS showed improved drug loading efficiency, release %age, and antioxidant activity compared to pure BS when loaded onto LCAg NPs. DLCAg exhibited excellent anti-inflammatory activity in rat models. These findings indicate that galloyl-BS (drug)-loaded LCAg (DLCAg) NPs have the potential as an anti-inflammatory agent without any prior release and scavenging in normal cells.


Asunto(s)
Lignina , Nanopartículas del Metal , Sitoesteroles , Ratas , Animales , Lignina/farmacología , Nanopartículas del Metal/química , Espectroscopía Infrarroja por Transformada de Fourier , Antiinflamatorios no Esteroideos/farmacología , Antioxidantes/farmacología , Antioxidantes/química , Antiinflamatorios/farmacología
2.
Langmuir ; 39(33): 11571-11581, 2023 Aug 22.
Artículo en Inglés | MEDLINE | ID: mdl-37549018

RESUMEN

Superhydrophobic cotton fabrics with multifunctional features are highly desired in domestic and outdoor applications. However, the short coating longevity and hazardous reagents significantly reduce their commercial-scale applications. Herein, we introduce CeO2 nanoparticles and stearic acid (SA) to develop a fluorine-free, durable superhydrophobic cotton fabric that mimics the lotus effect. The pristine cotton fabric is treated with APTES-functionalized CeO2 nanoparticles by immersion followed by a dip and drying treatment with a 2% myristic acid solution. This sequential process creates a stable superhydrophobic cotton fabric (SA/CeO2-cotton fabric) with a water contact angle of 158° and a water sliding angle of 5°. The results are attributed to the combined effect of CeO2 nanoparticles and stearic acid that enhances surface roughness and reduces surface sorption energy. APTES facilitates the durable attachment of CeO2 nanoparticles and stearic acid to the cotton fabric. The modified cotton fabric is characterized by advanced analytical tools, demonstrating enhanced superhydrophobicity, self-cleaning, and antiwater absorption properties. Additionally, it exhibits remarkable UV-blocking (UPF 542) and antibacterial properties. The designed superhydrophobic cotton fabric unveils good mechanical, thermal, and chemical durability. The proposed strategy is simple, green, and economical and can be used commercially for functional fabric preparation.

3.
J Sep Sci ; 45(23): 4236-4244, 2022 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-36168850

RESUMEN

Human serum N-linked glycans expression levels change during the disease progression. The low abundance, structural diversity, and coexisting matrices hinder their detection in mass spectrometry analysis. Considering the hydrophilic nature of N-glycans, cellulose/polymer (1,2-Epoxy-5-hexene) nanohybrid is fabricated with oxirane groups functionalized of asparagine to develop solid phase extraction based hydrophilic interaction liquid chromatography sorbent (cellulose/1,2-Epoxy-5-hexene/asparagine). The morphology, elemental analysis, and surface properties are studied through scanning electron microscopy, energy dispersive X-ray spectroscopy, and Fourier-transform infrared spectroscopy. The large surface area of cellulose/polymer nanohybrid (2.09 × 102  m2 /g) facilitates the high density of asparagine immobilization resulting in better hydrophilic interaction liquid chromatography enrichment under optimized conditions. The enrichment capability of nanohybrid/asparagine is assessed by the N-Linked glycans released from ovalbumin and immunoglobulin G where 23 and 13 N-glycans are detected respectively. The nanohybrid/asparagine shows selectivity of 1:1200 with spiked bovine serum albumin and sensitivity down to 100 attomole. Human serum profiling for N-glycans identifies 52 glycan structures. This new enrichment strategy enriches serum N-linked glycans in the presence of salts, proteins, endogenous serum peptides, and so forth.


Asunto(s)
Celulosa , Polímeros , Humanos , Asparagina
4.
Mikrochim Acta ; 189(8): 277, 2022 07 13.
Artículo en Inglés | MEDLINE | ID: mdl-35829791

RESUMEN

A new polymeric (methyl methacrylate/ethylene glycol dimethacrylate/1,2-epoxy-5-hexene) base/matrix has been fabricated and decorated with zwitterionic hydrophilic cysteic acid (Cya) for the enrichment of intact N-glycopeptides from standards and biological samples. Terpolymer-Cya provides good enrichment efficiency, improved hydrophilicity, and selectivity by virtue of better surface area (2.09 × 102 m2/g) provided by terpolymer and the zwitterionic property offered by cysteic acid. Cysteic acid-functionalized polymeric hydrophilic interaction liquid chromatography (HILIC) sorbent enriches 35 and 24 N-linked glycopeptides via SPE (solid phase extraction) mode from tryptic digests of model glycoproteins, i.e., immunoglobulin G (IgG) and horseradish peroxidase (HRP), respectively. Zwitterionic chemistry of cysteine helps in achieving higher selectivity with BSA digest (1:200), and lower detection limit down to 100 attomoles with a complete glycosylation profile of each standard digest. The recovery of 81% and good reproducibility define the application of terpolymer-Cya for complex samples like a serum. Analysis of human serum provides a profile of 807 intact N-linked glycopeptides via nano-liquid chromatography-tandem mass spectrometry (nLC-MS/MS). To the best of our knowledge, this is the highest number of glycopeptides enriched by any HILIC sorbent. Selected glycoproteins are evaluated in link to various cancers including the breast, lung, uterine, and melanoma using single-nucleotide variances (BioMuta). This study represents the complete idea of using an in-house developed strategy as a successful tool to help analyze, relate, and answer glycoprotein-based clinical issues regarding cancers.


Asunto(s)
Ácido Cisteico , Glicopéptidos , Glicopéptidos/análisis , Glicoproteínas , Humanos , Interacciones Hidrofóbicas e Hidrofílicas , Reproducibilidad de los Resultados , Espectrometría de Masas en Tándem
5.
Anal Bioanal Chem ; 413(30): 7441-7449, 2021 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-34686894

RESUMEN

Apo-H is a plasma glycoprotein. Nearly 19% of the molecular weight of this protein is composed of glycans. Up- and down-regulation and structural changes in protein glycans provide diagnostic value for disease detection. Here, an efficient, sensitive, and optimized method is developed for Apo-H N-glycans analysis by MALDI-TOF-MS in positive mode. This bioanalytical method includes sample preparation, sample purification, and detection. An Apo-H enrichment method is developed using standard proteins by anti-Apo-H beads followed by enrichment from plasma samples. SDS-PAGE confirms the Apo-H protein enrichment, which is further verified by LC-MS/MS analysis. The lower ionization efficiency of sialylated glycan hampers their analysis by MALDI-MS. For this, stabilization of sialic acids is done by selective derivatization of carboxyl groups to differentiate between α(2,3)- and α(2,6)-linked sialic acids. Glycans are further purified by HILIC-SPE and analyzed by MALDI-MS. Several branched bi- and tri-antennary glycans with fucosylation and sialylation are identified. The reproducibility of the developed method is tested by analyzing multiple replicates of human plasma, where the same glycans are consistently identified. This method could be applied for the Apo-H glycan profiling of large clinical cohorts for diagnostic purposes.


Asunto(s)
Ácido N-Acetilneuramínico/química , Polisacáridos/metabolismo , Espectrometría de Masa por Láser de Matriz Asistida de Ionización Desorción/métodos , beta 2 Glicoproteína I/metabolismo , Cromatografía Liquida/métodos , Estudios de Cohortes , Electroforesis en Gel de Poliacrilamida , Humanos , Reproducibilidad de los Resultados
6.
J Sep Sci ; 44(16): 3137-3145, 2021 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-34165915

RESUMEN

The surface of matrix-assisted laser desorption/ionization mass spectrometry target is modified for improved signal strength and detection of analytes. The developed method includes on-target enrichment and detection of phosphopeptides/phospholipids using graphene oxide-lanthanide metal oxides (samarium, gadolinium, dysprosium, and erbium) nanocomposites. Enriched phosphopeptides are detected using material enhanced laser desorption/ionization mass spectrometry and phospholipids by laser desorption/ionization-mass spectrometry. Nanocomposites are prepared using graphene oxide with respective metal salts at high pH. They are characterized for nano-morphology, chemistry, porosity, composition, crystallinity, and thermal stability. Phosphopeptides enrichment protocol is developed and optimized for tryptic ß-casein digest and that of phospholipids by phosphatidylcholine standard. Statistical analyses of phosphopeptides and phospholipids from milk show overlapping results for gadolinium, dysprosium, and erbium oxide nanocomposites. GO-Gd2 O3 has better enrichment efficiency and application as LDI material. Selectivity for GO-Dy2 O3 is 1:2500, for GO-Sm2 O3 is 1:3500, and 1:4000 for GO-Gd2 O3 . GO-Er2 O3 has a sensitivity of 25 fmol, whereas the highest sensitivity is down to 0.5 fmol for GO-Gd2 O3 . On-target enrichment is batch to batch reproducible with a standard deviation of <1, reduced time of enrichment to 10 min, and ease of operation compared to solid-phase batch extraction. The developed method enriches serum phosphopeptides characteristic of cancer-related phosphoproteins.


Asunto(s)
Materiales Biocompatibles/química , Grafito/química , Nanopartículas del Metal/química , Metales/química , Nanocompuestos/química , Óxidos/química , Animales , Caseínas/química , Bovinos , Humanos , Concentración de Iones de Hidrógeno , Espectrometría de Masas , Leche/química , Fosfolípidos/química , Fosfopéptidos/química , Fosforilación , Suero/química
7.
Mikrochim Acta ; 188(12): 417, 2021 11 11.
Artículo en Inglés | MEDLINE | ID: mdl-34762162

RESUMEN

A three-step strategy is introduced to develop inherent iminodiacetic (IDA)-functionalized nanopolymer. SEM micrographs show homogenous spherical beads with a particle size of 500 nm. Further modification to COOH-functionalized 1,2-epoxy-5-hexene/DVB mesoporous nanopolymer enriches glycopeptides via hydrophilic interactions followed by their MS determination. Significantly high BET surface area 433.4336 m2 g-1 contributes to the improved surface hydrophilicity which is also shown by high concentration of ionizable carboxylic acids, 14.59 ± 0.25 mmol g-1. Measured surface area is the highest among DVB-based polymers and in general much higher in comparison to the previously reported BET surface areas of co-polymers, terpolymers, MOFs, and graphene-based composites. Thirty-one, 19, and 16 N-glycopeptides are enriched/identified by nanopolymer beads from tryptic digests of immunoglobulin G, horseradish peroxidase, and chicken avidin, respectively, without additional desalting steps. Material exhibits high selectivity (1:400 IgG:BSA), sensitivity (down to 0.1 fmol), regeneration ability up to three cycles, and batch-to-batch reproducibility (RSD > 1%). Furthermore, from 1 µL of digested human serum, 343 N-glycopeptide characteristics of 134 glycoproteins including 30 FDA-approved serum biomarkers are identified via nano-LC-MS/MS. The developed strategy to self-generate IDA on polymeric surface with improved surface area, porosity, and ordered morphology is insignia of its potential as chromatographic tool contributing to future developments in large-scale biomedical glycoproteomics studies.


Asunto(s)
Glicopéptidos/química , Iminoácidos/química , Nanoestructuras/química , Polímeros/química , Humanos , Interacciones Hidrofóbicas e Hidrofílicas , Microscopía Electrónica de Rastreo , Nanoestructuras/ultraestructura , Porosidad , Propiedades de Superficie
8.
Mikrochim Acta ; 188(10): 338, 2021 Sep 12.
Artículo en Inglés | MEDLINE | ID: mdl-34510324

RESUMEN

An electrochemical sensor based on an antimony/nitrogen-doped porous carbon (Sb/NPC) composite has been developed for the quantitative detection of albumin from hepatocellular carcinoma (HCC) patients. Sb/NPC is hydrothermally synthesized from Sn/NPC precursors. The synthesized precursor (Sn/NPC) and the product (Sb/NPC) are characterized by XRD, FTIR, TGA, UV/Vis, SEM, and AFM. Cyclic voltammetry, chronoamperometry, and electrochemical impedance studies are used to investigate the electrochemical performance of Sb/NPC-GCE. Sb/NPC-GCE detects albumin at physiological pH of 7.4 in the potential range 0.92 V and 0.09 V for oxidation and reduction, respectively. LOD and recovery of Sb/NPC-GCE for the determination of albumin are 0.13 ng.mL-1 and 66.6 ± 0.97-100 ± 2.73%, respectively. Chronoamperometry of the modified working electrode demonstrates its stability for 14 h, indicating its reusability and reproducibility. Sb/NPC-GCE is a selective sensor for albumin detection in the presence of interfering species. The electrode has been applied for albumin detection in human serum samples of HCC patients. A negative correlation of albumin with alpha-fetoprotein levels in HCC patients is observed by statistical analysis.


Asunto(s)
Antimonio/química , Carbono/química , Carcinoma Hepatocelular/sangre , Neoplasias Hepáticas/sangre , Nitrógeno/química , Albúmina Sérica/análisis , Estaño/química , Técnicas Electroquímicas , Humanos , Albúmina Sérica/química
9.
Anal Chem ; 92(1): 683-689, 2020 01 07.
Artículo en Inglés | MEDLINE | ID: mdl-31840983

RESUMEN

Enrichment strategies are designed for the pretreatment of low-abundance glycans and glycopeptides prior to mass spectrometric (MS) analysis. Here, a tip-based strategy is being reported for the enrichment of glycopeptides and glycans using a piperazine modified polymeric monolithic tip. The tip is fabricated using the free radical polymerization. Fast separation (2 min) is achieved under optimized conditions with 20 cycles per step of loading, incubation, washing, and elution followed by MALDI-MS analysis. A total of 25, 22, and 34 glycopeptides covering all glycosylation sites are enriched by the modified tips from tryptic digests of horse radish peroxidase, chicken avidin, and human immunoglobulin G, respectively. Piperazine exhibits high selectivity 1:400 horse radish peroxidase/bovine serum albumin, sensitivity to 100 attomoles, recovery 89.51%, and batch to batch reproducibility (RSD > 1) in glycopeptides enrichment. Piperazine tips also enrich glycans from ovalbumin and human immunoglobulin G. High selectivity (1:1200, ovalbumin/BSA) and detection limit of 100 attomole is attained for glycans and furthermore 58 glycans are enriched from human serum. Thus, piperazine tips can be used as an enrichment tool for swift, cost-effective routine analysis of biological samples for separation of glycopeptides and glycans.


Asunto(s)
Glicopéptidos/sangre , Polímeros/química , Polisacáridos/sangre , Animales , Bovinos , Glicopéptidos/metabolismo , Peroxidasa de Rábano Silvestre/química , Peroxidasa de Rábano Silvestre/metabolismo , Humanos , Polisacáridos/metabolismo , Albúmina Sérica Bovina/química , Albúmina Sérica Bovina/metabolismo
10.
Anal Bioanal Chem ; 412(7): 1509-1520, 2020 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-32002580

RESUMEN

Highly specific enrichment of N-linked glycopeptides from complex biological samples is crucial prior to mass spectrometric analysis. In this work, a hydrophilic metal-organic framework composite is prepared by the growth of UiO-66-NH2 on graphene sheets, followed by its post-synthetic modification to attach boronic acid to form GO@UiO-66-PBA. The fabrication of graphene oxide-MOF composite results in enhanced surface area with improved thermal and chemical stability. The synthesized MOF nanocomposite is characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and BET. A crystalline structure with high porosity offering large surface area and good hydrophilicity of the nanocomposite assists as an enrichment tool in glycoproteomics. The GO@UiO-66-PBA nanocomposite selectively enriches N-linked glycopeptides from tryptic digests of horseradish peroxidase (HRP) and immunoglobulin (IgG). GO@UiO-66-PBA nanoparticles show a low detection limit (1 fmol) and good specificity (1:200), reusability and reproducibility for N-linked glycopeptide enrichment from IgG digest. The binding capacity of GO@UiO-66-PBA is 84 mg/g for protein concentration, with a good recovery of 86.5%. A total of 372 N-linked glycopeptides corresponding to different glycoproteins are identified from only 1 µL of human serum digest. Thus, the presented research work can be an efficient separation platform for N-linked glycopeptide enrichment from complex samples, which can be extended to cost-effective routine analysis. Graphical abstract.


Asunto(s)
Ácidos Borónicos/química , Glicopéptidos/química , Estructuras Metalorgánicas/química , Grafito/química , Peroxidasa de Rábano Silvestre/química , Humanos , Microscopía Electrónica de Rastreo , Reproducibilidad de los Resultados
11.
J Sep Sci ; 43(7): 1348-1355, 2020 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-31970866

RESUMEN

Enrichment of glycoproteins has been important because of their dynamicity and role in biological systems. Study of glycoproteins is complex because of the simultaneous glycosylation and deglycosylation inside the body. Often employed affinities for glycopeptides are hydrazide, boronic acid, or physiosorbed lectin on support materials. Cellulose, a natural polysaccharide, has rich surface chemistry, stable structure, low cost and availability in different variants. In present study, fibrous cellulose is oxidized using periodate to modify with boronic acid. Attachment of boronic acid is confirmed by Fourier transform infrared spectroscopy. Particle size and morphology of boronic acid@fibrous cellulose is studied by scanning electron microscopy. The enrichment efficiency is evaluated by using horseradish peroxidase as model protein. Boronic acid@fibrous cellulose is selective up to 1:250 for spiked horseradish peroxidase in bovine serum albumin digest, sensitive down to 0.1 femtomol and recovering 88.15% glycopeptides. Moreover, protein binding capacity is determined as 213 mg/g and 41% sequence coverage of horseradish peroxidase protein with all eight glycosylation sites detected. Total of 18 glycopeptides are enriched from immunoglobulin digest showing ability of boronic acid@fibrous cellulose to enrich glycoproteins from multiglycoforms. Enrichment from human serum recovers 18% extracellular and 72% secreted glycoproteins via bottom-up approach and online tools.


Asunto(s)
Ácidos Borónicos/metabolismo , Celulosa/metabolismo , Glicopéptidos/metabolismo , Adsorción , Animales , Ácidos Borónicos/sangre , Ácidos Borónicos/química , Bovinos , Celulosa/sangre , Celulosa/química , Glicopéptidos/sangre , Glicopéptidos/química , Peroxidasa de Rábano Silvestre/metabolismo , Humanos , Inmunoglobulinas/metabolismo , Albúmina Sérica Bovina/metabolismo , Espectrometría de Masa por Láser de Matriz Asistida de Ionización Desorción
12.
Biomed Chromatogr ; 34(1): e4693, 2020 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-31465544

RESUMEN

High-density lipoproteins (HDLs) have anti-inflammatory and antioxidant properties and are potentially cardio-protective. Defective HDL function is caused by alterations in both the proteome and lipidome of HDL particles. As potential biomarkers, the development of analytical methods is necessary for the enrichment of HDLs. Therefore, a method for selective enrichment of HDLs using immobilized metal ion affinity chromatography (IMAC) and metal oxide affinity chromatography (MOAC) is presented. SPE-based isolation of HDLs from whole serum is adopted as an alternative to traditional ultracentrifugation methods followed by SDS-PAGE. The enrichment mechanism relies on isoelectric points of lipoproteins and metal oxide. Negatively charged lipoprotein particles interact with positively charged metal oxides and IMAC affinity, which acts as a cation. Identified proteins from HDL through MALDI-MS analysis are apo AI, AII, AIV, CI, CIII, E, J, M, H, serum amyloid A and other nonapoproteins that are part of HDL particles and perform cellular functions. This serum-based proteomics approach gives insight into the functional role of HDL. HDL-associated phospholipids have also been analyzed by LDI-MS. Results suggest that the adopted analytical strategy is a feasible idea to extract lipoproteins from serum. A comparative study of healthy and diseased samples using this approach will provide valuable information in future.


Asunto(s)
Cromatografía de Afinidad/métodos , Lipoproteínas HDL/sangre , Fosfolípidos/sangre , Proteoma/análisis , Humanos , Lipoproteínas HDL/aislamiento & purificación , Fosfolípidos/aislamiento & purificación , Espectrometría de Masa por Láser de Matriz Asistida de Ionización Desorción
13.
Mikrochim Acta ; 187(10): 555, 2020 09 10.
Artículo en Inglés | MEDLINE | ID: mdl-32910214

RESUMEN

A hydrophilic terpolymer MOF composite is designed with high surface area and porosity to enrich mono- and multi-glycosylated peptides facilitating a bottom-up approach. Terpolymer@ZIF-8 is synthesized using free radical polymerization followed by layer by layer ZIF-8 fabrication. Subsequent surface modification was made by aminophenylboronic acid (AMBA). The enrichment ability of terpolymer@ZIF-8@BA is evaluated by using tryptic digest of IgG and HRP to exemplify mono- and multi-glycosylated protein samples. Improved selectivity of 1:200 for spiked HRP in BSA digest and sensitivity down to 1 fmol µL-1 is achieved. Batch to batch reproducibility is better 1% RSD which favors the adoption of the developed method for routine N-linked glycopeptide/protein determination. Cost-effective nature of given approach is given by regeneration of the material up to four cycles. Total 318 N-linked glycopeptides have been identified from 1 µL human serum digest after subjecting the enriched and PNGase-treated deglycosylated peptides to LC-MS. Thus, terpolymer@ZIF-8@BA holds the potential both for mono- and multi-glycosylated peptides from complex biological sample. Graphical abstract.


Asunto(s)
Glicopéptidos/metabolismo , Espectrometría de Masas/métodos , Péptidos/metabolismo
14.
Anal Bioanal Chem ; 411(9): 1745-1759, 2019 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-30680427

RESUMEN

Metal-organic frameworks (MOFs) are an eminent addition to materials science research because of their versatile properties due to which their applications are wide spread in proteomics. They are used in various fields due to their characteristics like higher surface area, specific symmetry, ease of modification, and availability of a variety of ligands. As affinity sorbents, they have shown higher selectivity, sensitivity, and reproducibility than conventionally used materials. They are applied for the enrichment of phosphopeptides, glycopeptides, low mass peptides, and as laser desorption/ionization (LDI) matrices for small-molecule analysis. This review captures the insight of applying MOFs in the field of mass spectrometry-based proteomics. The specific features are discussed regarding MOFs as affinity sorbents for the selective capture of biological molecules like phosphopeptides and glycopeptides from complex samples. The potential of MOFs as LDI mass spectrometry (LDI-MS) matrices for small-molecule analysis is also evaluated. MOFs have also been used as enzymatic reactors for the digestion of proteins, prior to MS analysis. MOF-based affinity materials and bioreactors reduce proteome complexity and improve detection sensitivity and coverage. Size-exclusion effects of MOFs help in subtracting the abundant proteins in peptidomics. Several limitations of MOFs are addressed, which include stability under varying pH conditions, the unclear interaction mechanism between the MOFs and targeted analytes, and the non-specific binding that interferes during the analysis because of metal centers and ligands in the MOFs. This will open up MOF-based research to overcome the limitations and improve the performance of MOFs as selective and sensitive materials. Graphical abstract ᅟ.


Asunto(s)
Estructuras Metalorgánicas , Proteómica , Ligandos
15.
Anal Bioanal Chem ; 411(15): 3373-3382, 2019 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-31016328

RESUMEN

Titania-grafted magnetic sporopollenin is synthesized by the liquid-phase deposition (LPD) technique, characterized by SEM, EDX, and nitrogen adsorption porosimetry, and used for the selective enrichment of phosphorylated peptides. The material is low cost because of easier availability of pollens and has rich surface chemistry which enables strong attachment of titania onto magnetic sporopollenin. The material shows higher selectivity of 1:1000 with ß-casein spiked in BSA. Higher sensitivity of 10 fmol is recorded for phosphopeptides from standard ß-casein digest. Twenty phosphorylated peptides are enriched from milk digest and four endogenous phosphopeptides from diluted human serum. The magnetic property of titania-coated magnetic sporopollenin facilitates the fast and effective isolation of phosphopeptides from complex mixtures through external magnet. The material is finally applied to tryptic digest of rat brain cell lysate for phosphopeptide enrichment where 2718 phosphopeptides are identified by using LC-MS/MS with C18 column. Titania-coated magnetic sporopollenin captures both mono-phosphorylated (2489) and multi-phosphorylated peptides (229) due to strong affinity of TiO2 with phosphates. TiO2-coated magnetic material also shows better enrichment efficiency in comparison to commercial TiO2. Graphical abstract.


Asunto(s)
Biopolímeros/química , Química Encefálica , Carotenoides/química , Imanes/química , Fosfopéptidos/análisis , Titanio/química , Adsorción , Animales , Carotenoides/síntesis química , Caseínas/química , Bovinos , Magnetismo/métodos , Fosfopéptidos/aislamiento & purificación , Ratas , Albúmina Sérica Bovina/química , Espectrometría de Masa por Láser de Matriz Asistida de Ionización Desorción/métodos
16.
Mikrochim Acta ; 186(12): 852, 2019 11 28.
Artículo en Inglés | MEDLINE | ID: mdl-31776681

RESUMEN

An anion exchange solid-phase sorbent is described. Chitosan coated magnetite nanoparticles were modified with polyethylenimine which is positively charged at pH 3 and therefore can be used for the magnet-supported enrichment of phosphopeptides which are negatively charged at this pH value. A 2-step strategy was used to synthesize the sorbent. The materials were characterized by transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, thermogravimetry and magnetic moment analysis. The anion exchanger was applied to extract phosphopeptides from a ß-casein digest. Characteristic analytical figures include (a) a loading buffer of pH 3, (b) and elution buffer of pH 11, (c) a loading time of 5 min, (d) good selectivity (the ß-casein to BSA ratio is 1:1000), and (e) excellent sensitivity (1 fmol). The optimized method was applied to egg yolk digest, non-fat milk digest, and diluted human serum. Graphical abstractSchematic representation of synthesis of PEI@chitosan@Fe3O4 nanoparticles, and of the enrichment of phosphopeptides by magnetic solid phase extraction prior to the determination of the peptides by MALDI-MS analysis.


Asunto(s)
Quitosano/química , Nanopartículas de Magnetita/química , Fosfopéptidos/aislamiento & purificación , Polietileneimina/química , Adsorción , Animales , Aniones/química , Bovinos , Yema de Huevo/química , Humanos , Leche/química , Tamaño de la Partícula , Fosfopéptidos/sangre , Fosfopéptidos/química , Propiedades de Superficie
17.
World J Microbiol Biotechnol ; 35(12): 188, 2019 Nov 18.
Artículo en Inglés | MEDLINE | ID: mdl-31741120

RESUMEN

Soil contamination due to cadmium (Cd) is a ubiquitous environmental problem for which inexpensive remediation alternatives are required. Phytoaccumulation, the use of plants to extract and accumulate heavy metals from the contaminated environment, is such an alternative. In this study, we aimed at establishing effective plant-bacteria interplay between Brachiaria mutica and Cd-resistant endophytic bacteria eventually leading to improved phytoremediation. B. mutica was grown in a Cd-contaminated soil and inoculated with three Cd-tolerant endophytic bacteria individually as well as in combination. Plant physiological parameters, biomass production, bacterial colonization, and Cd-accumulation were observed at four different Cd exposures, i.e., 100, 200, 400 and 1000 mg kg-1 of soil. The combined application of endophytic bacteria was more effective as compared to their individual applications at all concentrations. Nevertheless, highest performance of consortium was seen at 100 mg Cd kg-1 of soil, i.e., root length was enhanced by 46%, shoot length by 62%, chlorophyll content by 40%, and dry biomass by 64%; which was reduced with the increase in Cd concentration. The bacterial population was highest in the root interior followed by rhizosphere and shoot interior. Concomitantly, plants inoculated with bacterial consortium displayed more Cd-accumulation in the roots (95%), shoots (55%), and leaves (44%). Higher values of BCFroot (> 1), and lower values for BCFshoot and TF (< 1) indicates capability of B. mutica to accumulate high amounts of Cd in the roots as compared to the aerial parts. The present study concludes that plant-endophyte interplay could be a sustainable and effective strategy for Cd removal from the contaminated soils.


Asunto(s)
Brachiaria/metabolismo , Brachiaria/microbiología , Cadmio/metabolismo , Endófitos/fisiología , Bacterias/metabolismo , Biodegradación Ambiental , Biomasa , Brachiaria/efectos de los fármacos , Brachiaria/crecimiento & desarrollo , Cadmio/análisis , Cadmio/farmacología , Productos Agrícolas , Metales Pesados , Hojas de la Planta/metabolismo , Raíces de Plantas/microbiología , Brotes de la Planta/metabolismo , Brotes de la Planta/microbiología , Rizosfera , Suelo/química , Microbiología del Suelo , Contaminantes del Suelo
18.
Analyst ; 143(23): 5610-5628, 2018 Nov 19.
Artículo en Inglés | MEDLINE | ID: mdl-30411734

RESUMEN

Cerium-based materials possess redox properties due to the presence of dual valence states of Ce3+ and Ce4+. In the last few years, the scientific community has paid much attention to designing and synthesizing cerium-based materials through advantageous routes for widespread catalytic and sensing applications in many fields. Cerium materials have been synthesized in many different forms, shapes and sizes. The catalytic and sensing capabilities of cerium nanostructures are highly dependent on their morphologies and can be improved significantly by modifying the sizes and shapes of the nanostructures to develop sensing scaffolds with improved sensing performance. These nanostructures provide a basis for applications in many fields. From a literature survey (2010 to 2015), it can be concluded that the fundamental morphologies, ratios, and capping of cerium nanostructures (CeNSs) constructively affect their properties and applications. Designed sensors utilizing CeNSs exhibit outstanding stability, high selectivity and eminent reproducibility in relation to time and temperature. This review will provide a perspective insight on the future trends in the design of different morphologies of CeNSs and their promising applications.

19.
Anal Chem ; 89(19): 10232-10238, 2017 10 03.
Artículo en Inglés | MEDLINE | ID: mdl-28849910

RESUMEN

Polymeric monoliths fabricated in tips with embedded materials of choice are important in separation science. Polymeric backbone however interferes in the enrichment and thus affects efficiency. This work focuses on the in-tip fabrication of lanthanum oxide porous monolith and its application in the enrichment of phosphorylated peptides and lipids. Polycondensation reaction uses an aqueous solution of LaCl3·7H2O with N-methyl formamide as porogen and propylene oxide as initiator. The aging time of monolith and temperature condition for the reaction are optimized to attain porous monolithic tip. A comparison of (i) solid phase batch extraction using La2O3, (ii) La2O3 embedded in poly(glycidyl methacrylate (GMA)/divinylbenzene (DVB)) tip, and (iii) pure La2O3 monolithic tip shows improved enrichment efficiency in the case of pure La2O3 monolithic tip. The monolithic tip achieves selectivity of 1:4500 as compared to solid phase extraction (SPE)(1:3500) and limit of detection down to 0.25 fmol. The in-tip La2O3 monolith strategy has better batch to batch reproducibility, reduced time of enrichment, and ease of operation in comparison to solid phase batch extraction. The developed strategy enriches phospho- content from biological samples like phosvitin and lipovitellin from egg yolk and phospholipids/phosphopeptides from human serum. The enriched phospho- moieties are analyzed by matrix-assisted laser desorption ionization-mass spectrometry (MALDI-MS) except the phospholipids where laser desorption ionization (LDI)-MS is employed.


Asunto(s)
Lantano/química , Óxidos/química , Fosfolípidos/análisis , Fosfopéptidos/análisis , Espectrometría de Masa por Ionización de Electrospray , Espectrometría de Masa por Láser de Matriz Asistida de Ionización Desorción , Proteínas del Huevo/análisis , Yema de Huevo/metabolismo , Compuestos Epoxi/química , Humanos , Límite de Detección , Fosfolípidos/sangre , Fosfolípidos/aislamiento & purificación , Fosfopéptidos/sangre , Fosfopéptidos/aislamiento & purificación , Fosvitina/análisis , Polímeros/química , Porosidad , Extracción en Fase Sólida , Compuestos de Vinilo/química
20.
Biochem Biophys Res Commun ; 482(4): 615-624, 2017 Jan 22.
Artículo en Inglés | MEDLINE | ID: mdl-27865835

RESUMEN

Super-activation of cholinesterases (acetylcholinesterase and butyrylcholinesterase) are linked to various neurological problems most precisely Alzheimer's disease (AD), which leads to senile dementia. Therefore, cholinesterases (AChE & BChE) inhibition are considered as a promising strategy for the treatment of Alzheimer's disease. FDA approved drugs for the treatment of AD, belong to a group of cholinesterase inhibitors. However, none of them is able to combat or completely abrogate the disease progression. Herein, we report a series of newly synthesized chalcone derivatives with anti-AD potential. For this purpose, a series of piperidyl-thienyl and 2-pyrazoline derivatives of chalcones were tested for their cholinesterases (AChE & BChE) inhibitory activity. All compounds were found as selective inhibitor of AChE. In piperidyl chalcones derivatives compound 1e having IC50 of 0.16 ± 0.008 µM and 2m in 2-pyrazoline chalcones with IC50 of 0.13 ± 0.006 µM, were found to be the most potent inhibitors of AChE, exhibiting ≈142 and ≈ 173-fold greater inhibitory potential compared to the reference inhibitor i.e., Neostigmine (IC50 ± SEM = 22.2 ± 3.2 µM). Molecular docking studies of most potent inhibitors were carried out to investigate the binding interactions inside the active site. Molecular docking study revealed that potent compounds and co-crystalized ligand had same binding orientation within the active site of target enzyme. Most of these compounds are selective inhibitors of AChE with a potential use against progressive neurodegenerative disorder and age related problems.


Asunto(s)
Acetilcolinesterasa/metabolismo , Butirilcolinesterasa/metabolismo , Chalconas/química , Chalconas/farmacología , Inhibidores de la Colinesterasa/química , Inhibidores de la Colinesterasa/farmacología , Enfermedad de Alzheimer/tratamiento farmacológico , Enfermedad de Alzheimer/enzimología , Animales , Electrophorus , Humanos , Simulación del Acoplamiento Molecular , Pirazoles/química , Pirazoles/farmacología
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