RESUMEN
Development of a multifunctional sensor is highly desirable. In this work, traces of a carcinoid cancer biomarker of 5-hydroxyindole-3-acetic acid (5-HIAA) in real human urine can be detected by lanthanide nanoparticle Eu-CFC (CFC = 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid) and the sensing devices of the test paper and agarose gel, achieving an ultralow LOD of 0.8 × 10-3 ppm within a sensing time of 2.0 min. Interestingly, by metal center regulation of Tb and Eu codoping, nanoparticle TbEu2-CFC shows high-sensitivity and low-LOD (0.019% v/v) sensing of water in ethanol. The sensing mechanisms are revealed by both experiments and quantum chemical studies.
RESUMEN
With the continuous development of industrialization, the excessive emission of nitro aromatic with strong toxicity, high carcinogenicity and non-degradability has attracted great attention. How to efficiently remove nitro aromatic pollutants is an important research topic. In this work, graphene oxide/covalent organic frameworks (GO/COFs) composites were successfully synthesized via interlayer confinement strategy selecting GO, 2,5-dimethoxybenzene-1,4-dicarboxaldehyde (DMTP) and 1,3,5-tri(4-aminophenyl)benzene (TPB) as raw materials. Due to high specific surface area, hierarchical porous structure and good thermal stability, GO/COFs were utilized to adsorb and remove nitro aromatic hydrocarbons in the water environment. The adsorption behavior of GO/COFs for o-nitrophenol, 1,3-dinitrobenzene and 2,4,6-trinitrophenol were further investigated. The GO/COFs composites showed the strongest adsorption capacity for 2,4,6-trinitrophenol, and the maximum adsorption capacity for 2,4,6-trinitrophenol, o-nitrophenol, and 1,3-dinitrobenzene were 438, 317, and 173 mg g-1, respectively. The experimental results indicated that the GO/COFs composites provided great adsorption capability for nitro aromatic pollutants and can be reused, rendering it an extremely potential adsorbent for organic pollutants.
Asunto(s)
Grafito , Contaminantes Químicos del Agua , Adsorción , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/aislamiento & purificación , Grafito/química , Nitrofenoles/química , Nitrofenoles/aislamiento & purificación , Estructuras Metalorgánicas/química , Purificación del Agua/métodosRESUMEN
Tetracycline (TC) as a broad-spectrum antibiotic, is widely used in the prevention and treatment of various bacterial diseases. However, its abuse in the livestock industry may lead to interference in human microecology, thereby causing various side effects. In this study, deep eutectic solvents (DESs) were synthesized using L-(-)-threonine (L-(-)-Thr) and cerium nitrate hexahydrate (Ce(NO3)3·6H2O), and later lanthanum nitrate hexahydrate (La(NO3)3·6H2O) was doped to synthesize La-Ce hybrid nanorods. These nanorods can be used for the determination of TC with high sensitivity and selectivity by the colorimetric method. This approach has a linear response to TC between 0.05 µM and 10 µM, with a detection limit of 0.016 µM. In this system, good dispersion provides the substance with a distinct peroxidase activity, which is used to create a colorimetric sensor for detecting TC. Mechanism studies show that the superoxide radical generated by the La-Ce nanomembrane plays a key role in peroxidase catalysis. Finally, the practicality of the method was verified by the determination of TC in food products (milk, pork and honey), which demonstrated that a good recovery rate can be obtained (91.4-102%).
Asunto(s)
Cerio , Colorimetría , Lantano , Leche , Nanotubos , Tetraciclina , Colorimetría/métodos , Nanotubos/química , Lantano/química , Cerio/química , Tetraciclina/análisis , Tetraciclina/química , Leche/química , Animales , Miel/análisis , Disolventes Eutécticos Profundos/química , Análisis de los Alimentos/métodos , Límite de Detección , Contaminación de Alimentos/análisis , Antibacterianos/análisis , PorcinosRESUMEN
Chiral enantiomers, especially the enantiomers of chiral drugs often exhibit different pharmacological activity, metabolism and toxicity, thus it is of great research significance to scientifically and reasonably develop single chiral drugs with low toxicity and high efficiency. Among them, high performance liquid chromatographic techniques based on chiral stationary phases (CSPs) has become one of the most attractive methods used to evaluate the enantiomeric purity of single-enantiomers compound of pharmacological relevance. In this work, pillar[5]arene functionalized with L- and D-histidine, respectively, were modified on the surface of mesoporous silica as novel chiral stationary phases called L/DHis-BP5-Sil. Notably, L/D-histidine had the characteristics of low steric hindrance and easy derivatization. Although the π-π interaction of imidazole group was weaker than that of benzene ring, the benzene ring bonding imidazole-conjugated ring in the structure produced better enantioseparation effect. The results showed that L/DHis-BP5-Sil can separate a variety of complex structural enantiomers with excellent reproducibility, thermal stability and separation performance. Hence, the unique advantage of the highly selective separation of L/DHis-BP5-Sil provides new insights into the enantioseparation field.
Asunto(s)
Calixarenos , Histidina , Dióxido de Silicio , Estereoisomerismo , Dióxido de Silicio/química , Calixarenos/química , Histidina/química , Cromatografía Líquida de Alta Presión/métodos , Porosidad , Reproducibilidad de los Resultados , Compuestos de Amonio Cuaternario/químicaRESUMEN
In this paper, three imidazole- and C18- bifunctional silica stationary phases (Sil-Im-C18) were prepared by adjusting introduction interval of octadecyltrichlorosilane (ODS) and 3-imidazol-1-ylpropyl(trimethoxy)silane (TMPImS), which can be used for reversed-phase liquid chromatography (RPLC) and ion exchange chromatography (IEC) with adjustable performance. The successful preparation of Sil-Im-C18 were confirmed by the characterizations of elemental analysis, infrared spectroscopy (FTIR) and contact angle (CA). Chromatographic performance of Sil-Im-C18 were evaluated by the separation of Tanaka test mixture, alkylbenzenes, linear PAHs and a set of analytes with different properties (uracil, phenol, 1,2-dinitrobenzene and naphthalene), and compared with commonly used C18 column. It was found that the chromatographic performance of Sil-Im-C18 changed significantly with the difference in bonding amount of imidazole and C18. Sil-Im-C18 demonstrated the excellent separation performance towards polycyclic aromatic hydrocarbons (PAHs), phenylesters, phenylamines, phenols and inorganic anions, and notably, nucleobases and nucleosides can be separated using pure water as mobile phases. The van Deemter plot showed that the column efficiency of Sil-Im-C18-3 was 64,933 plate·m-1 for naphthalene, indicated that Sil-Im-C18 was reasonably chromatographic columns. The RSD values of retention time were 0.22 %-0.61 % for 10 needles alkylbenzenes injected continuously at 50 °C to investigate thermal stability and repeatability, all the fluctuations of k of naphthalene were less than 2.3 % for Sil-Im-C18-1 during flushing 24 h with the mobile phase at different pH values (pH = 3 and 8), the retention time of alkylbenzenes were almost same for Sil-Im-C18-1 at different time, the RSD values of retention time of alkylbenzenes were 0.45 %-2.28 % for two batches Sil-Im-C18-1, revealing the excellent repeatability, thermal stability, durability and reproducibility of Sil-Im-C18, and implying a commercial prospect.
Asunto(s)
Cromatografía de Fase Inversa , Imidazoles , Hidrocarburos Policíclicos Aromáticos , Dióxido de Silicio , Imidazoles/química , Dióxido de Silicio/química , Cromatografía de Fase Inversa/métodos , Hidrocarburos Policíclicos Aromáticos/análisis , Hidrocarburos Policíclicos Aromáticos/aislamiento & purificación , Hidrocarburos Policíclicos Aromáticos/química , Silanos/química , Cromatografía por Intercambio Iónico/métodosRESUMEN
Chiral pillar[5]arene-based mesoporous silica, an emerging class of chiral structure, possesses excellent characteristics such as abundant chiral active sites, encapsulated cavity and excellent chiral modification, which make them a promising candidate as new chiral stationary phases (CSPs) in enantioseparation. In this study, two imidazole-containing (S)-1-(4-phenyl-1H-imidazol-2-yl)ethanamine and (S)-Histidinol were respectively modified to bromoethoxy pillar[5]arene-bonded silica to construct new chiral stationary phases (sPIE-BP5-Sil and sHol-BP5-Sil) for the separation and analysis of enantiomers. The separation conditions such as mobile phase composition, flow rate and temperature were optimized. Under optimal conditions, both sPIE-BP5-Sil and sHol-BP5-Sil showed good separation performance for different types of enantiomers. Interestingly, sPIE-BP5-Sil and sHol-BP5-Sil showed better enantioselectivity for chiral aromatic compounds and chiral aliphatic compounds, respectively. This enantioseparation result was closely related to the presence of additional aromatic rings and abundant hydroxyl groups in the side chains of the two chiral groups. In addition, the enantioseparation process was further studied by molecular docking simulation. Therefore, this work provided a new strategy for the preparation and application of imidazolyl-derived pillar[5]arene-based chiral stationary phases, which can be efficiently used for screening and separating enantiomers.
Asunto(s)
Dióxido de Silicio , Cromatografía Líquida de Alta Presión , Dióxido de Silicio/química , Simulación del Acoplamiento Molecular , Estereoisomerismo , TemperaturaRESUMEN
Enantioselective discrimination of chiral molecules is essential in chemistry, biology, and medical science due to the configuration-dependent activities of enantiomers. Therefore, identifying a specific amino acid and distinguishing it from its enantiomer by using nanomaterials with outstanding performance are of great significance. Herein, blue- and green-emitting chiral silicon nanoparticles named bSiNPs and gSiNPs, respectively, with excellent water solubility, salt resistance, pH stability, photobleaching resistance, biocompatibility, and ability to promote soybean germination, were fabricated in a facile one-step method. Especially, chiral gSiNPs presented excellent fluorescence recognition ability for glutamic acid enantiomers within 1 min, and the enantiomeric recognition difference factor was as high as 9.0. The mechanism for enantiomeric fluorescence recognition was systematically explored by combining the fluorescence spectra with density functional theory (DFT) calculation. Presumably, the different Gibbs free energy and hydrogen-bonding interaction of the chiral recognition module with glutamic acid enantiomers mainly contributed to the difference in the fluorescence signals. Most noteworthy was the fact that the chiral gSiNPs can showcase not only the ability to recognize l- and d-glutamic acids in living cells but also the test strips fabricated by soaking gSiNPs can be applied for d-glutamic acid visual detection. As a result, this study provided insights into the design of multifunctional chiral sensing nanoplatforms for enantiomeric detection and other applications.
Asunto(s)
Ácido Glutámico , Nanopartículas , Silicio , Estereoisomerismo , Aminoácidos/química , Nanopartículas/química , ColorantesRESUMEN
In China, Jiang Fructus aurantii (JFA) has attracted increasing interest as a famous traditional herbal medicine and valuable economic food for its valuable medicinal and industrial properties. In the current work, contrasted with conventional extraction techniques, natural flavonoids from JFA (naringin and neohesperidin) were extracted with remarkable effectiveness utilizing a sustainable deep eutectic solvents combined ultrasonic-assisted extraction (DESs-UAE) protocol. The optimal extraction capacity can be achieved by mixing 30 % water with a molar ratio of 1:3 for choline chloride and ethylene glycol, as opposed to the classical extraction solvents of 95 % ethanol, methanol, and water. Moreover, the DESs-UAE extraction programs were also systematically optimized employing Box-Behnken design (BBD) trials, and the eventual findings suggested that the best parameters were a 27 % water content in DES, a 16 mL/g liquid-solid ratio, a 72 min extraction time, and a 62 °C extraction temperature, along with the corresponding greatest contents of NAR (48.18 mg/g) and NEO (34.50 mg/g), respectively. Notably, by comparison with the pre-optimization data, the optimized DES extraction efficiency of flavonoids is markedly higher. Thereafter, the characterization of the solvents before and after extraction, as well as the differences between the four extraction solvent extracts, were compared using the FT-IR analyses. Furthermore, SEM results suggested that the penetration and erosion abilities of the plant cell wall of DES-1 were stronger than those of the other three traditional solvents, thus allowing more release of flavonoid compounds. In conclusion, the present research develops a straightforward, sustainable, and exceedingly efficient approach for the extraction of bioactive flavonoids from JFA, which has the potential to facilitate the efficient acquisition of active ingredients from TCM.
Asunto(s)
Disolventes Eutécticos Profundos , Flavonoides , Flavonoides/análisis , Espectroscopía Infrarroja por Transformada de Fourier , Ultrasonido , Solventes , Agua , Extractos VegetalesRESUMEN
Enzyme activity assays play a crucial role in numerous fields, including biotechnology, the food industry, and clinical diagnostics. Lipases are particularly important enzymes due to their widespread use in lipid metabolism and esterification reactions. Here, we present a pioneering method for the sensitive and selective determination of lipase activity using green carbon dots (G-CDs) for first time. G-CDs are a fascinating class of carbon nanomaterials with unique optical properties and biocompatibility, making them ideal candidates for enzyme activity assays. This approach eliminates the need for traditional fluorophores or chromogenic substrates, reducing costs, fast response time (1 min), and environmental impact with a quantum yield (QY) of 7.42%. As designed, the G-CDs fluorescent probe turn-on demonstrated a reliable linear detection range from 0 to 9 mg/mL under ideal conditions, with detection limit of 0.01 mg/mL and limit of quantification (LOQ) of 0.045 mg/mL, respectively. Furthermore, the G-CDs system was thoroughly evaluated in human serum samples, showing recoveries ranging from 100.0 to 105.0%. These findings highlight the promising applicability of the G-CDs probe for lipase detection, yielding highly favorable results.
Asunto(s)
Colorantes Fluorescentes , Puntos Cuánticos , Humanos , Colorantes Fluorescentes/química , Carbono/química , Lipasa , Puntos Cuánticos/química , Espectrometría de FluorescenciaRESUMEN
The escalating prevalence of cephalosporin antibiotics in wastewater poses a serious threat to public health and environmental balance. Thus, it is crucial to develop effective methods for removing cephalosporin antibiotics from water sources. Herein, we propose the use of AuPtRh trimetallic nanoparticles supported on Ti3C2MXene as a photocatalyst for the degradation of cephalosporin antibiotics. Initially, AuPtRh nanoparticles were uniformly grown onto Ti3C2MXene sheets using one-step reduction technique. The prepared AuPtRh/Ti3C2MXene exhibited a complete degradation of cefixime and ceftriaxone sodium, while an impressive degradation efficiency of 91.58 % for cephalexin was achieved after 60 min of exposure to visible light, surpassing the performance of its individual AuPtRh nanoparticles and Ti3C2MXene. The enhanced photoactivity of AuPtRh/Ti3C2MXene was resulted from improved light absorption capacity and efficient generation, separation, and transfer of charge carriers driven by the formation of heterojunction between AuPtRh and Ti3C2MXene. Electron paramagnetic resonance and radicals trapping experiments results revealed that â¢O2- and h+ are the principal reactive species governing the degradation of cephalosporins. The photocatalyst exhibited excellent stability and could be reused four times without significant loss in efficiency. Our study highlights the potential of MXene composites for environmental remediation, offering insights into designing sustainable AuPtRh/Ti3C2MXene photocatalyst for water pollutant degradation.
Asunto(s)
Cefalosporinas , Nanopartículas , Nitritos , Elementos de Transición , Titanio , Cefalexina , LuzRESUMEN
Lung cancer is a malignant tumor with one of the highest morbidity and mortality rates in the world. Approximately 80-85% of lung cancer is diagnosed as non-small lung cancer (NSCLC), and its 5-year survival rate is only 21%. Cisplatin is a commonly used chemotherapy drug for the treatment of NSCLC. Its efficacy is often limited by the development of drug resistance after long-term treatment. Therefore, determining how to overcome cisplatin resistance, enhancing the sensitivity of cancer cells to cisplatin, and developing new therapeutic strategies are urgent clinical problems. Z-ligustilide is the main active ingredient of the Chinese medicine Angelica sinensis, and has anti-tumor activity. In the present study, we investigated the effect of the combination of Z-ligustilide and cisplatin (Z-ligustilide+cisplatin) on the resistance of cisplatin-resistant lung cancer cells and its mechanism of action. We found that Z-ligustilide+cisplatin decreased the cell viability, induced cell cycle arrest, and promoted the cell apoptosis of cisplatin-resistant lung cancer cells. Metabolomics combined with transcriptomics revealed that Z-ligustilide+cisplatin inhibited phospholipid synthesis by upregulating the expression of phospholipid phosphatase 1 (PLPP1). A further study showed that PLPP1 expression was positively correlated with good prognosis, whereas the knockdown of PLPP1 abolished the effects of Z-ligustilide+cisplatin on cell cycle and apoptosis. Specifically, Z-ligustilide+cisplatin inhibited the activation of protein kinase B (AKT) by reducing the levels of phosphatidylinositol 3,4,5-trisphosphate (PIP3). Z-ligustilide+cisplatin induced cell cycle arrest and promoted the cell apoptosis of cisplatin-resistant lung cancer cells by inhibiting PLPP1-mediated phospholipid synthesis. Our findings demonstrate that the combination of Z-Ligustilide and cisplatin is a promising approach to the chemotherapy of malignant tumors that are resistant to cisplatin.
Asunto(s)
Cisplatino , Neoplasias Pulmonares , Humanos , Cisplatino/farmacología , Cisplatino/uso terapéutico , Neoplasias Pulmonares/tratamiento farmacológico , Neoplasias Pulmonares/genética , Neoplasias Pulmonares/metabolismo , 4-Butirolactona/farmacología , Fosfolípidos/farmacología , Resistencia a Antineoplásicos/genética , Apoptosis , Línea Celular Tumoral , Proliferación CelularRESUMEN
Covalent organic frameworks (COFs) stand for a class of emerging crystalline porous organic materials, which are ingeniously constructed with organic units through strong covalent bonds. Their excellent design capabilities, and uniform and tunable pore structure make them potential materials for various applications. With the continuous development of synthesis technique and nanoscience, COFs have been successfully combined with a variety of functional materials to form COFs-based composites with superior performance than individual components. This paper offers an overview of the development of different types of COFs-based composites reported so far, with particular focus on the applications of COFs-based composites. Moreover, the challenges and future development prospects of COFs-based composites are presented. We anticipate that the review will provide some inspiration for the further development of COFs-based composites.
RESUMEN
A novel C4-modified bipyridinium stationary phase (Sil-DPC4) was prepared and characterized by elemental analysis (EA) and Fourier transform infrared spectrometry (FT-IR) and further investigated for multi-mode liquid chromatography. The chromatographic performances of Sil-DPC4 were evaluated by reversed-phase chromatography using polycyclic aromatic hydrocarbons (PAHs), phenylamines and phenols, hydrophilic interaction chromatography using nucleosides and nucleobases, and ion exchange chromatography using inorganic ions and organic ions. The effects of the acetonitrile content, salt concentration and pH value of the mobile phase on the retention of Sil-DPC4 were also investigated. Sil-DPC4 showed multiple retention mechanisms including π-π, hydrophobic and electrostatic interactions for PAHs, phenylamines and phenols compared with a dipyridine modified silica stationary phase (Sil-DP) and C18 in RPLC, faster separation for nucleosides and nucleobases compared with Sil-DP, and higher hydrophilicity than HILIC in HILIC, and stronger retention and better separation ability for inorganic ions and organic ions in comparison to Sil-DP in IEC. Besides, Sil-DPC4 was used successfully to detect iodide in artificial seawater and had the potential to analyze radionuclide iodine-131 in seawater. In conclusion, multiple retention mechanisms of Sil-DPC4 could make it have potential applications in complex samples.
RESUMEN
Chromatographic column is the core of chromatographic separation, and chromatographic separation material is considered the soul of the chromatographic column. The type and characteristics of the chromatographic separation material directly determine the separation mode and performance of chromatographic columns. The development and preparation of separation materials with novel structures and good separation performance is an ongoing hotspot in chromatography research. Given rapid developments in nanoscience and technology, nanomaterials with unique surface functional groups and large specific surface areas have attracted extensive attention and great interest from researchers in the field of separation science. Carbon dots (CDs), a new type of zero-dimensional fluorescent carbon nanomaterials, have been widely used in bioimaging, light-emitting diodes, sensing, catalysis, drug delivery, and other applications since they were first reported in 2004. These nanomaterials present several advantages over other types of separation materials, including a simple preparation process, low toxicity, easy functionalization, excellent biocompatibility, and photobleaching resistance. In addition, compared with traditional carbon nanomaterials such as graphene and carbon nanotubes, CDs have abundant surface functional groups, nanoscale sizes, and moderate adsorption properties. Hence, when CDs-based new materials are applied as a stationary phase for column chromatography, they can provide rich reaction sites and ensure the uniformity of the chromatographic packing process. The use of CDs can effectively avoid the peak-tailing phenomenon caused by the strong interaction of large π-conjugated systems with some analytes and improve the efficiency of the chromatographic column. As such, these nanomaterials show good application prospects in the field of chromatographic separation. In this review, the development history, classification, and synthesis strategies of CDs are briefly described. We then focus on the development of CDs-based chromatographic separation materials by systematically reviewing the recent advances in the use of CDs-based materials as a stationary phase for high-performance liquid chromatography (including hydrophilic interaction, reversed-phase, mixed-mode, and chiral chromatography), gas chromatography, and capillary electrochromatography, with special emphasis on the preparation methods and applications of various stationary phases. Finally, the development prospects of CDs and future research efforts on these materials are also analyzed and discussed. This review can provide guidance on the rational design and application of new CDs-based chromatographic separation materials.
RESUMEN
Chirality is a common phenomenon in nature. Different enantiomers of chiral drug compounds have obvious differences in their effects on the human body. Therefore, the separation of chiral drugs plays an extremely important role in the safe utilization of drugs. High-performance liquid chromatography (HPLC) is an effective tool for the separation and analysis of compounds, in which the chromatographic packing plays a key role in the separation. Chiral pharmaceutical separation and analysis in HPLC rely on chiral stationary phases (CSPs). Thus, various CSPs are being developed to meet the needs of chiral drug separation and analysis. In this review, recent developments in CSPs, including saccharides (cyclodextrin, cellulose, amylose and chitosan), macrocycles (macrocyclic glycopeptides, pillar[n]arene and polyamide) and porous organic materials (metal-organic frameworks, covalent organic frameworks, and porous organic cages), for pharmaceutical analysis in HPLC were summarized, the advantages and disadvantages of various stationary phases were introduced, and their development prospects were discussed.
Asunto(s)
Amilosa , Estructuras Metalorgánicas , Humanos , Cromatografía Liquida , Cromatografía Líquida de Alta Presión , Celulosa , Preparaciones FarmacéuticasRESUMEN
As a typical chronic inflammatory joint disease with swelling and pain syndromes, rheumatoid arthritis (RA) is closely related to articular lubrication deficiency and excessive proinflammatory cytokines in its progression and pathogenesis. Herein, inspired by the dual effects of joint lubrication improvement and anti-inflammation to treat RA, two novel potential therapeutic nanoagents have been developed rationally by employing herbal medicine-derived carbon quantum dots (CQDs), i.e., safflower (Carthamus tinctorius L.) CQDs and Angelica sinensis CQDs, yielding ultrahigh lubrication and anti-inflammation bioefficacy. In vitro experimental results show that the two nanoagents display excellent friction reduction due to their good water solubility and spherical structure. Using RA rat models, it is indicated that the nanoagents significantly relieved swelling symptoms and inhibited the expression of related inflammatory cytokines, including IL-1, IL-6, and TNF-α, indicating their extraordinary anti-inflammation bioefficacy. Thus, combining the lubricating and anti-inflammation bioefficacy of CQDs derived from herbal medicine is an attractive strategy to develop new nanoagents for RA treatment.
Asunto(s)
Artritis Reumatoide , Medicamentos Herbarios Chinos , Puntos Cuánticos , Ratas , Animales , Carbono/uso terapéutico , Lubrificación , Puntos Cuánticos/uso terapéutico , Artritis Reumatoide/tratamiento farmacológico , Antiinflamatorios/farmacología , Antiinflamatorios/uso terapéutico , Citocinas/metabolismo , Medicamentos Herbarios Chinos/farmacología , Medicamentos Herbarios Chinos/uso terapéuticoRESUMEN
In this work, tetraethylenepentamine (TEPA) was used as precursor and reaction medium to prepare tetraethylenepentamine-functionalized carbon dots (TEPACDs), the resultant mixture was subsequently silanized and then grafted on the surface of bare silica. The obtained tetraethylenepentamine-functionalized carbon dots and tetraethylenepentamine co-modified silica stationary phase (Sil-TEPA/CDs) was characterized by multiple ways, such as Fourier transformed infrared spectroscopy (FTIR), elemental analysis and transmission electron microscope, which revealed the successful preparation of the mixed stationary phase and higher density of functional groups on co-modified stationary phase than precursor single-modified stationary phase. The synergistic effect of TEPACDs and TEPA was proved by comparing the separation performance of Sil-TEPA/CDs and Sil-TEPA toward amino acids, nucleosides, and nucleobases, which distinctly enhanced the selectivity of Sil-TEPA/CDs. Thus, 12 nucleosides and nucleobases and 11 amino acids was nicely separated on Sil-TEPA/CDs. By study the influences of the changes of mobile phase composition, mobile phase buffer concentration and buffer pH on the retention behaviors of Sil-TEPA and Sil-TEPA/CDs, it was found that both hydrophilic partitioning and adsorption of analytes on Sil-TEPA/CDs were enhanced benefit from the co-existence of TEPA and TEPACDs, which provided the analytes better separation performance. By comparing the column quality of Sil-TEPA/CDs with four commercially available columns, Sil-TEPA/CDs exhibited the best peak asymmetry of 0.98, and second best column efficiency of 43895 m-1 using guanosine as analyte. The RSD (n = 9) of the retention times of five selected analytes on Sil-TEPA/CDs were within 0.30-0.61% during 40 h of continuously elution, which implied excellent stability of prepared packing material.
Asunto(s)
Aminoácidos , Nucleósidos , Carbono , Cromatografía , Dióxido de Silicio , TrietilenofosforamidaRESUMEN
Ionic liquids (ILs), which are salts in a molten state below 100 °C, have become a hot topic of research in various fields because of their negligible vapour pressure, high thermal stability, and tunable viscosity. Chiral ionic liquids (CILs) can be applied in chromatography and capillary electrophoresis fields to improve the performance of enantiomeric separation, such as chiral stationary phases (CSPs) and mobile phase additives in high-performance liquid chromatography (HPLC); CSPs in gas chromatography (GC); and background electrolyte additives (BGE), chiral ligands and chiral selectors (CSs) in capillary electrophoresis (CE). This review focuses on the applications of CILs in HPLC and CE for the separation of enantiomers in the past five years. The mechanism for separating enantiomers was explained, and the prospect of the application of CILs in chiral liquid chromatography (LC) and CE analysis was also discussed.
RESUMEN
Mn3O4 nanoparticles composed of porous reduced graphene oxide nanosheets (Mn3O4@p-rGO) with enhanced oxidase-like activity were successfully fabricated through an in-situ approach for fast colorimetric detection of ascorbic acid (AA). The residual Mn2+ in the GO suspension of Hummers method was directly reused as the manganese source, improving the atom utilization efficiency. Benefiting from the uniform distribution of Mn3O4 nanoparticles on the surface of p-rGO nanosheets, the nanocomposite exhibited larger surface area, more active sites, and accelerated electron transfer efficiency, which enhanced the oxidase-like activity. Mn3O4@p-rGO nanocomposite efficiently activate dissolved O2 to generate singlet oxygen (1O2), leading to high oxidation capacity toward the substrate 3,3',5,5'-tetramethylbenzidine (TMB) without the extra addition of H2O2. Furthermore, the prominent absorption peak of the blue ox-TMB at 652 nm gradually decreased in the presence of AA, and a facile and fast colorimetric sensor was constructed with a good linear relationship (0.5-80 µM) and low LOD (0.278 µM) toward AA. Owing to the simplicity and excellent stability of the sensing platform, its practical application for AA detection in juices has shown good feasibility and reliability compared with HPLC and the 2, 4-dinitrophenylhydrazine colorimetric method. The oxidase-like Mn3O4@p-rGO provides a versatile platform for applications in food testing and disease diagnosis.