RESUMEN
Panax quinquefolius (PQ) has been widely used in traditional Chinese medicine and functional food. Ginsenosides are the important functional components of PQ. The ginsenosides' diversity is deeply affected by the processing conditions. The ginsenosides in the steamed PQ have been not well-characterized yet because of the complexity of their structure. In the study, the comprehensive investigation of ginsenosides was performed on the steamed PQ with different steaming times and temperatures by UPLC-Q-TOF-MS. Based on the molecular weight, retention time and characterized fragment ions, 175 ginsenosides were unambiguously identified or tentatively characterized, including 45 protopanaxatriol type, 49 protopanaxadiol type, 19 octillol type, 6 oleanolic acid type ginsenosides, and 56 other ginsenosides. Ten new ginsenosides and three new aglycones were discovered in the steamed PQ samples through searching the database of CAS SciFindern. Principal component analysis showed the significant influence on the chemical components of PQ through different processing conditions. The steaming temperature was found to promote the transformation of ginsenosides more than the steaming time. The protoginsenosides were found to transform into the rare ginsenosides by elimination reactions. The malonyl ginsenosides were degraded into acetyl ginsenosides, and then degraded into neutral ginsenosides. The sugar chain experienced degradation, with position changes and configuration inversions. Furthermore, 20 (S/R)-ginsenoside Rh1, Rh2, Rg2, and Rh12 were found to transform from the S-configuration to the R-configuration significantly. This study could present a comprehensive ginsenosides profile of PQ with different steaming conditions, and provide technical support for the development and utilization of PQ.
Asunto(s)
Ginsenósidos , Panax , Ginsenósidos/química , Cromatografía Líquida con Espectrometría de Masas , Panax/química , Cromatografía Liquida , Espectrometría de Masas en Tándem , Vapor , Cromatografía Líquida de Alta PresiónRESUMEN
The practical catalytic enantioselective cis-dihydroxylation of olefins that utilize earth-abundant first-row transition metal catalysts under environmentally friendly conditions is an important yet challenging task. Inspired by the cis-dihydroxylation reactions catalyzed by Rieske dioxygenases and non-heme iron models, we report the biologically inspired cis-dihydroxylation catalysis that employs an inexpensive and readily available mononuclear non-heme manganese complex bearing a tetradentate nitrogen-donor ligand and aqueous hydrogen peroxide (H2O2) and potassium peroxymonosulfate (KHSO5) as terminal oxidants. A wide range of olefins are efficiently oxidized to enantioenriched cis-diols in practically useful yields with excellent cis-dihydroxylation selectivity and enantioselectivity (up to 99% ee). Mechanistic studies, such as isotopically 18O-labeled water experiments, and density functional theory (DFT) calculations support that a manganese(V)-oxo-hydroxo (HO-MnVâO) species, which is formed via the water-assisted heterolytic O-O bond cleavage of putative manganese(III)-hydroperoxide and manganese(III)-peroxysulfate precursors, is the active oxidant that effects the cis-dihydroxylation of olefins; this is reminiscent of the frequently postulated iron(V)-oxo-hydroxo (HO-FeVâO) species in the catalytic arene and alkene cis-dihydroxylation reactions by Rieske dioxygenases and synthetic non-heme iron models. Further, DFT calculations for the mechanism of the HO-MnVâO-mediated enantioselective cis-dihydroxylation of olefins reveal that the first oxo attack step controls the enantioselectivity, which exhibits a high preference for cis-dihydroxylation over epoxidation. In this study, we are able to replicate both the catalytic function and the key chemical principles of Rieske dioxygenases in mononuclear non-heme manganese-catalyzed enantioselective cis-dihydroxylation of olefins.
Asunto(s)
Dioxigenasas , Peróxido de Hidrógeno/química , Manganeso , Oxidación-Reducción , Alquenos/química , Estereoisomerismo , Hierro/química , Oxidantes , Catálisis , AguaRESUMEN
The quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach is widely used in sample pretreatment in agricultural products, food, environment, etc. And nano-materials are widely used in QuEChERS method due to its small size and large specific surface area. In this review, we examine the typical applications of several commonly used nano-materials in improved QuEChERS method. These materials include multi-walled carbon nanotubes (MWCNTs) and their derivatives, magnetic nanoparticles (MNPs), metal organic frameworks (MOFs), covalent organic frameworks (COFs), graphene oxide (GO), lipid and protein adsorbent (LPAS), cucurbituril (CBs), and carbon nano-cages (CNCs), and so on. The strengths and weaknesses of each nano-material are presented, as well as the challenging aspects that need to be addressed in future research. By comparing the applications and the current technology development, this review suggests utilizing artificial intelligence (AI) to screen suitable combinations of purification agents and performing virtual simulation experiments to verify the reliability of this methodology. By doing so, we aim to accelerate the development of new products and decrease the cost of innovation. It also recommends designing smarter pretreatment instruments to enhance the convenience and automation of the sample pretreatment process and reduce the margin for human error.
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To efficiently eliminate highly polar organic pollutants from water has always been a difficult issue, especially in the case of ultralow concentrations. Herein, we present the facile synthesis of quinolinecarboxylic acid-linked COF (QCA-COF) via the Doebner multicomponent reaction, possessing multifunction, high specific surface area, robust physicochemical stability, and excellent crystallinity. The marked feature lies in the quinolinyl and carboxyl functions incorporated simultaneously to QCA-COF in one step. The major cis-orientation of carboxyl arms in QCA-COF was speculated by powder X-ray diffraction and total energy analysis. QCA-COF demonstrates excellent adsorption capacity for water-soluble organic pollutants such as rhodamine B (255.7 mg/g), methylene blue (306.1 mg/g), gentamycin (338.1 mg/g), and 2,4-dichlorophenoxyacetic acid (294.1 mg/g) in water. The kinetic adsorptions fit the pseudo-second order model and their adsorption isotherms are Langmuir model. Remarkably, QCA-COF can capture the above four water-soluble organic pollutants from real water samples at ppb level with higher than 95% removal efficiencies and excellent recycling performance.
RESUMEN
In this paper, an imine-based porous 3D covalent organic polymer (COP) was synthesized via solvothermal condensation. The structure of the 3D COP was fully characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and powder X-ray diffractometry, thermogravimetric analysis, and Brunauer-Emmer-Teller (BET) nitrogen adsorption. This porous 3D COP was used as a new sorbent for the solid-phase extraction (SPE) of amphenicol drugs, including chloramphenicol (CAP), thiamphenicol (TAP), and florfenicol (FF) in aqueous solution. Factors were investigated for their effects on the SPE efficiency, including the types and volume of eluent, washing speed, pH, and salinity of water. Under the optimized conditions, this method gave a wide linear range (0.1-200 ng/mL) with a high correlation coefficient value (R2 > 0.99), low limits of detection (LODs, 0.01-0.03 ng/mL), and low limits of quantification (LOQs, 0.04-0.10 ng/mL). The recoveries ranged from 83.98% to 110.7% with RSDs ≤ 7.02%. The good enrichment performance for this porous 3D COP might contribute to the hydrophobic and π-π interactions, the size-matching effect, hydrogen bonding, and the good chemical stability of 3D COP. This 3D COP-SPE method provides a promising approach to selectively extract trace amounts of CAP, TAP, and FF in environmental water samples in ng quantities.
RESUMEN
Pb2+ pollution and poisoning are serious environmental and pharmacological concerns. The World Health Organization reported that Pb has resulted in 540,000 deaths in 2016 alone. Therefore, effective drugs or supplements that can alleviate or offset Pb2+-induced toxicity are badly needed. Through screening biocompatible natural compounds, we discovered that chicoric acid exhibited potent protective activities against Pb2+-induced toxicity both in BV-2 microglial cells and in zebrafish from the first days of development. Chicoric acid was able to reduce Pb2+-induced increases in levels of reactive oxygen species and tumor necrosis factor alpha, restoring the cell cycle in BV-2â¯cells. In the zebrafish model, chicoric acid significantly alleviated the Pb2+-induced serious mortality and malformation of zebrafish larvae in a concentration-dependent manner. These protective activities of chicoric acid were mainly from its alleviation of Pb2+-induced dysregulation of oxidative response pathways, including key genes such as Aox1, Gclm, Hmox1, Nqo1, Scd1, and Srxn1, as well as HO-1 protein. Since Pb2+ is difficult to be completely eliminated from the body and chelating agents may cause serious adverse effects, chicoric acid is likely a potential supplement therapy, in addition to current clinical practices.
Asunto(s)
Ácidos Cafeicos/farmacología , Contaminantes Ambientales/toxicidad , Larva/efectos de los fármacos , Plomo/toxicidad , Microglía/efectos de los fármacos , Estrés Oxidativo/efectos de los fármacos , Succinatos/farmacología , Pez Cebra/metabolismo , Animales , Antioxidantes/metabolismo , Línea Celular , Supervivencia Celular/efectos de los fármacos , Hemo-Oxigenasa 1/metabolismo , Larva/metabolismo , Ratones , Especies Reactivas de Oxígeno/metabolismo , Pruebas de ToxicidadRESUMEN
Metal-organic coordination polymer beads (MOCBs) are described for use as a sorbent for solid-phase extraction of chlorophenoxy herbides. By applying regulation of Co(II) ions, micro-sized monodisperse MOCBs were obtained through the microwave heating. The MOCBs-based method displays excellent extraction efficiency towards chlorophenoxy herbicides, specifically of 2-chlorophenoxyacetic acid, 4-chlorophenoxyacetic acid, 4-chloromethylphenoxyacetic acid, 2,4-dichlorophenoxyacetic acid, 2,4,5-trichlorophenoxyacetic acid and 2-(2,4-dichlorophenoxy)propionic acid. Following extraction, the herbicides were eluted with 8% formic acid in methanol and quantified by HPLC. The method, when applied to analyze spiked cereals, exhibits a wide linear range (from 0.6 to 1000 ng g-1) and low limits of quantification (ranging from 0.10 to 0.25 ng g-1). For a single column, the inter-day and intra-day precisions, expressed as the relative standard deviation are in the range of 2.5-6.8%. The batch-to-batch reproducibility (for n = 3) is <4.6%. For spiked cereal samples, relative recoveries are very good (90.3-102.3%, for n = 4). The extraction efficiency of MOCBs remains unchanged after reusing for 40 times. Graphical abstractSchematic presentation of Co(II)-doped metal-organic coordination polymer beads (Co(II)@MOCB) using for solid-phase extraction (SPE).
Asunto(s)
Ácido 2,4-Diclorofenoxiacético/análogos & derivados , Ácido 2,4-Diclorofenoxiacético/aislamiento & purificación , Herbicidas/aislamiento & purificación , Estructuras Metalorgánicas/química , Extracción en Fase Sólida/métodos , Ácido 2,4-Diclorofenoxiacético/análisis , Adsorción , Cromatografía Líquida de Alta Presión , Cobalto/química , Grano Comestible/química , Contaminación de Alimentos/análisis , Herbicidas/análisis , Herbicidas/química , Límite de Detección , Magnoliopsida/química , Estructuras Metalorgánicas/síntesis química , Reproducibilidad de los ResultadosRESUMEN
The authors describe a new spherical metal-organic coordination polymer (MOCP) for use as an adsorbent in solid-phase microextraction (SPME). By applying the ions Co(II), Fe(II), Cu(II), and Zn(II) in these polymers, MOCP with different morphology were obtained. The respective coatings for SPME display different extraction efficiency towards neonicotinoid insecticides (neo-nics). The Co(II)@MOCP coating displays an improved extraction capability for neo-nics when compared to the four commercially available coatings studied. Following extraction with the Co(II)@MOCP-coated fiber, the neo-nics were eluted using 1 mL of trifluoroacetic acid/acetonitrile solution and quantified by high performance liquid chromatography. The method, when applied to spiked honey samples, has good linearity (0.5-600 µg kg-1) and a low limit of detection (0.05-0.15 µg kg-1). The precision (n = 6) for a single fiber was in the range of 3.6-8.3%. The reproducibility (for n = 5) from fiber-to-fiber ranges between 5.4 and 8.8%. The Co(II)@MOCP-coated fiber can be reused more than 80 times without any apparent reduction in its performance. In addition, the relative recoveries from spiked honey samples are very good (91.5%-103.5%). Graphical abstract A spherical metal-organic coordination polymer (MOCP) was synthesized under the regulation of Co(II) and used for the solid-phase microextraction (SPME) of neonicotinoid insecticides found in honey.
RESUMEN
An efficient analytical method based on molecularly imprinted solid-phase extraction (MISPE) coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) was established for the determination of iridoid glycosides (IGs) in Di-huang pills. As the solid-phase extraction medium, superhydrophilic molecularly imprinted polymers (MIPs) with high affinity and selectivity to IGs in water media were fabricated using divinyl galactose as a single cross-linking monomer. The structure, porosity, and hydrophilicity of MIPs were characterized. The properties involving dynamic adsorption, kinetic adsorption, and selectivity were evaluated. Under optimal conditions the MISPE-HPLC-DAD based method was applied for loganin, morroniside, cornin, and sweroside determination in three kinds of Di-huang pills. The limits of detection of four IGs were 0.002-0.003 mg g-1. Furthermore, the proposed method exhibited some merits including good linearity, excellent precision, and desirable accuracy. The established MISPE-HPLC-DAD method has great potential for the selective determination of IGs in Chinese patent drugs. Graphical Abstract á .
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Reactivos de Enlaces Cruzados/química , Glicósidos Iridoides/análisis , Preparaciones Farmacéuticas/análisis , Polímeros/química , Adsorción , Interacciones Hidrofóbicas e Hidrofílicas , Glicósidos Iridoides/química , Límite de Detección , Impresión Molecular/métodos , Estructura Molecular , Preparaciones Farmacéuticas/química , Extracción en Fase Sólida/métodos , Agua/químicaRESUMEN
Molecularly imprinted covalent organic polymers were constructed by an imine-linking reaction between 1,3,5-triformylphloroglucinol and 2,6-diaminopyridine and used for the selective solid-phase extraction of benzoxazole fluorescent whitening agents from food samples. Binding experiments showed that imprinting sites on molecularly imprinted polymers had higher selectivity for targets compared with those of the corresponding non-imprinted polymers. Parameters affecting the solid-phase extraction procedure were examined. Under optimal conditions, actual samples were treated and the eluent was analyzed with high-performance liquid chromatography with diode-array detection. The results showed that the established method has a wide linearity, satisfactory detection limits and quantification limits, and acceptable recoveries. Thus, this developed method possesses the practical potential for the selective determination of benzoxazole fluorescent whitening agents in complex food samples.
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Benzoxazoles/aislamiento & purificación , Colorantes Fluorescentes/aislamiento & purificación , Contaminación de Alimentos/análisis , Impresión Molecular , Polímeros/química , Agaricales/química , Benzoxazoles/química , Cromatografía Líquida de Alta Presión , Harina/análisis , Colorantes Fluorescentes/química , Estructura Molecular , Extracción en Fase SólidaRESUMEN
Five iridoid glycosides were prepared using molecularly imprinted solid-phase extraction combined with preparative high-performance liquid chromatography. Hydrophilic molecularly imprinted polymers were synthesized using α-1-allyl-2-N-acetyl glucosamine, which introduced an abundance of hydrophilic groups into the polymers. Using molecularly imprinted solid-phase extraction as the sample pretreatment procedure, five iridoid glycosides, gardenoside, geniposide, shanzhiside, geniposidic acid, and genipin-1-O-gentiobioside, were selectively enriched from Gardenia fructus extracts. Preparative high-performance liquid chromatography then provided iridoid glycosides with a purity >98%. The structures were elucidated by using nuclear magnetic resonance spectroscopy, optical rotation and melting point measurements, and mass spectrometry. The results demonstrate that molecularly imprinted solid-phase extraction combined with preparative high-performance liquid chromatography was an efficient, rapid, and economical method for the preparation of bioactive compounds from natural products.
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/aislamiento & purificación , Gardenia/química , Glicósidos Iridoides/aislamiento & purificación , Polímeros/química , Extracción en Fase Sólida/métodos , Medicamentos Herbarios Chinos/química , Interacciones Hidrofóbicas e Hidrofílicas , Glicósidos Iridoides/química , Impresión Molecular , Polímeros/síntesis química , Extracción en Fase Sólida/instrumentaciónRESUMEN
High-speed counter-current chromatography (HSCCC) coupled with precolumn derivatization was developed for isolating and purifying fructo-oligosaccharides (FOSs). Firstly, the total FOSs were precolumn derivatized and then separated by high-speed counter-current chromatography (HSCCC) with two-phase solvent system petroleum ether-n-butanol-methanol-water (3:2:1:4, v/v). Secondly, the obtained compounds were deacetylated and the fructo-oligosaccharides (FOSs) with high purity were obtained. Their structures were identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). This research successfully established a novel strategy for separation and purification of FOS. There is no doubt that the application of the research will be beneficial for the quantitative and qualitative analysis of products containing FOSs.
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Oligosacáridos/aislamiento & purificación , 1-Butanol/química , Alcanos/química , Cromatografía Líquida de Alta Presión , Distribución en Contracorriente , Espectroscopía de Resonancia Magnética , Espectrometría de Masas , Metanol/química , Estructura Molecular , Oligosacáridos/química , Oxidación-Reducción , Solventes/química , Agua/químicaRESUMEN
We describe a solid-phase extraction adsorbent based on molecularly imprinted polymers (MIPs), prepared with use of a mimic template. The MIPs were used for the selective extraction and determination of three chlorogenic acids as combined quality markers for Lonicera japonica and Lianhua qingwen granules. The morphologies and surface groups of the MIPs were assessed by scanning electron microscopy, Brunauer-Emmett-Teller surface area analysis, and Fourier transform infrared spectroscopy. The adsorption isotherms, kinetics, and selectivity of the MIPs were systematically compared with those of non-molecularly imprinted polymers. The MIPs showed high selectivity toward three structurally similar chlorogenic acids (chlorogenic acid, cryptochlorogenic acid, and neochlorogenic acid). A procedure using molecularly imprinted solid-phase extraction coupled with high-performance liquid chromatography was established for the determination of three chlorogenic acids from Lonicera japonica and Lianhua qingwen granules. The recoveries of the chlorogenic acids ranged from 93.1% to 101.4%. The limits of detection and limits of quantification for the three chlorogenic acids were 0.003 mg g-1 and 0.01 mg g-1, respectively. The newly developed method is thus a promising technique for the enrichment and determination of chlorogenic acids from herbal medicines. Graphical Abstract Mimic molecularly imprinted polymers for the selective extraction of chlorogenic acids.
Asunto(s)
Ácido Clorogénico/química , Medicamentos Herbarios Chinos/química , Lonicera/química , Polímeros/química , Adsorción , Impresión Molecular , Estructura Molecular , Control de CalidadRESUMEN
Hydrophilic molecularly imprinted polymers (H-MIP) with molecular recognition ability for iridoid glycosides (IGs) have been obtained via bulk polymerization combined with hydrolysis of ester groups. H-MIP were characterized by Fourier transform infrared spectroscopy (FT-IR). The hydrophilcity was measured by the contact angle measurement and the water dispersion stability. The obtained H-MIP demonstrated high selectivity and specific binding ability to five IGs in aqueous media. The group extraction efficiency of molecular imprinted solid-phase extraction (MISPE) for five IGs was investigated, including loading sample, breakthrough volume, washing solvent, and elution solvent. Compared with non-imprinted solid-phase extraction (NISPE), the higher average recovery (95.5 %) of five IGs with lower relative standard deviations values (below 6.1 %) using MISPE combined with high-performance liquid chromatography (HPLC) were achieved at three spiked levels in three blank samples. Under the optimum MISPE conditions, the wide linear range with the correlation coefficient of R (2) ≥ 0.9950 for five IGs with low limits of detection (LOD) and quantification (LOQ) (0.01-0.08 and 0.03-0.27 µg mL(-1), respectively) were obtained. Chromatograms obtained using MISPE columns demonstrated that the matrix interference has been minimized and great interferences around IGs were also eliminated efficiently. These results indicated that the developed MISPE-HPLC method was selective, accurate, and applicable for the determination of IGs in water media. Graphical Abstract Preparation of hydrophilic molecularly imprinted polymers via bulk polymerization combined with hydrolysis of ester groups.
RESUMEN
In this work, dummy molecularly imprinted polymers with high selectivity and affinity to capsaicin and dihydrocapsaicin are designed using N-vanillylnonanamide as a dummy template. The performance of dummy molecularly imprinted polymers and nonimprinted polymers was evaluated using adsorption isotherms, adsorption kinetics, and selective recognition capacity. Dummy molecularly imprinted polymers were found to exhibit good site accessibility, taking just 20 min to achieve adsorption equilibrium; they were also highly selective toward capsaicin and dihydrocapsaicin. We successfully used dummy molecularly imprinted polymers as a specific sorbent for selectively enriching capsaicin and dihydrocapsaicin from chili pepper samples. In a scaled-up experiment, the selective recovery of capsaicinoids was calculated to be 77.8% using solid-phase extraction. To the best of our knowledge, this is the first example of the use of N-vanillylnonanamide as a dummy template in molecularly imprinted polymers to simultaneously enrich capsaicin and dihydrocapsaicin.
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Capsaicina/análogos & derivados , Capsaicina/aislamiento & purificación , Capsicum/química , Extractos Vegetales/aislamiento & purificación , Polímeros/química , Extracción en Fase Sólida/métodos , Adsorción , Capsaicina/química , Impresión Molecular , Extractos Vegetales/química , Polímeros/síntesis química , Extracción en Fase Sólida/instrumentaciónRESUMEN
Aflatoxin B1 (AFB1) is a common mycotoxin that is of significant global concern due to its impact on food safety. Herein, we innovatively develop a sensing platform to detect AFB1 based on evaporation of surfactant solutions on the hydrophobic surface, resulting in dried patterns with varied sizes. The surfactant CTAB solution produces a relatively large dried pattern due to the surface wetting. However, the reduction in the dried pattern size is found when the mixture of CTAB and AFB1 aptamer is tested, because the formation of CTAB/aptamer complex. Moreover, the dried pattern size of the mixture of CTAB, aptamer, and AFB1 increases due to the specific binding of AFB1 to its aptamer. Using this innovative strategy, the AFB1 detection can be fulfilled with a detection limit of 0.77 pg/mL. As a simple, convenient, inexpensive, and label-free method, the surfactant-mediated surface droplet evaporation-based biosensor is very promising for various potential applications.
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Aflatoxina B1 , Técnicas Biosensibles , Contaminación de Alimentos , Tensoactivos , Aflatoxina B1/análisis , Aflatoxina B1/química , Tensoactivos/química , Técnicas Biosensibles/instrumentación , Técnicas Biosensibles/métodos , Contaminación de Alimentos/análisis , Límite de Detección , Aptámeros de Nucleótidos/química , Interacciones Hidrofóbicas e HidrofílicasRESUMEN
Herein, burdock polysaccharide (BP) and modified burdock polysaccharide (MBP) were prepared, followed by the fabrication of chlorogenic acid (CA)-BP, CA-MBP, isochlorogenic acid A (ICA)-BP, and ICA-MBP nanoparticles. Afterward, the structural characteristics, physical stability, digestive characteristics, and antioxidant activity of hydrogen peroxide (H2O2)-damaged HepaRG cells were evaluated. The result indicated that the loading capacities of CA in BP-CA and MBP-CA were 0.14 and 0.53 µg/mg, respectively. Conversely, the loading capacities of ICA in BP-ICA and MBP-ICA were 0.36 and 0.60 µg/mg, respectively. Four complex nanoparticles exhibited excellent physical stability under different pH values, temperatures, and ionic concentrations, especially MBP-CA and MBP-ICA. Moreover, four complex nanoparticles could protect caffeoylquinic acid from being released in gastric fluid. All six samples exhibited high antioxidant activity in H2O2-induced HepaRG cells, especially BP and MBP-CA. These findings indicated that caffeoylquinic acid-polysaccharide complexes were successfully prepared and highlighted the potential of polysaccharides as natural carriers for hydrophobic bioactive molecules.
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Per- and polyfluoroalkyl substances (PFASs) can lead to risks associated with animal and human health through the transfer along food chains. It is confirmed that PFASs can be transported to each part of plants after taken up by the roots. To better elucidate the underlying mechanisms for such exposure, it is highly valuable to develop analytical capabilities for in vivo monitoring of PFASs in live plants. In this work, a novel imprinted covalent organic frameworks (CMIP) solid-phase microextraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry was developed with low limits of detection for six acidic PFASs (0.1-0.3 ng g-1) and used for in vivo monitoring in live aloe. The CMIP coating shows good precision (RSD of intra and inter ≤9.6 % and 10.2 %, respectively) and possesses much higher extraction efficiency than the commercial coatings. After cultivating aloe in soil spiked PFASs, the in vivo assays gave a wealth of information, including steady-state concentrations, translocation factors, elimination rate constants, and half-life of PFASs. The in vivo tracing method for live plants can provide much needed and unique information to evaluate the risk of PFASs, which are very important for the safety of agriculture production.
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Aloe , Fluorocarburos , Estructuras Metalorgánicas , Humanos , Animales , Cromatografía Líquida de Alta Presión/métodos , Aloe/química , Microextracción en Fase Sólida , Fluorocarburos/análisisRESUMEN
Aflatoxins (AFs) exhibit hepatotoxicity, immunotoxicity, and carcinogenicity, and their detection in food has attracted widespread concern. An ordered macroporous metal-organic framework (OM-ZIF-8) based on solid-phase extraction (SPE) was used to extract six AFs from milk products. The SPE conditions, including eluting solvent, eluting volume, amounts of OM-ZIF-8, pH of loading solution, loading solvent, ionic strength, loading flow rate, and elution flow rate, were exhaustively optimized. Under optimal parameters, the six AFs were detected by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The OM-ZIF-8 exhibited satisfactory AFs extraction performance through ordered macropore structure, π-π interaction, coordination interaction, and electrostatic interaction. Furthermore, linearity in the range of 0.01-100 ng mL-1 with low detection limits of 0.002-0.0150 ng mL-1 was obtained, and the relative recoveries of AFs were 80.3-110 % with relative standard deviation ≤8.7 %. Thus, this research provides a promising platform for the analysis of trace AFs in complex foods.
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Aflatoxinas , Estructuras Metalorgánicas , Animales , Leche/química , Aflatoxinas/análisis , Espectrometría de Masas en Tándem/métodos , Extracción en Fase Sólida/métodos , Cromatografía Líquida de Alta Presión/métodos , Solventes/análisisRESUMEN
The precise determination of polypeptide antibiotics (PPTs) in foods has been always challenging because of the interference of various endogenous peptides in complex matrix. Herin, a novel large-pore covalent organic framework (TABPT-SPDA-COF) with accessible pore size of 7.9 nm was synthesized as a solid phase extraction (SPE) absorbent for efficiently enriching four PPTs existed in foods originating from animals. The parameters of SPE process were systematically optimized. Subsequently, four PPTs were determined by UHPLC-MS/MS. Under the optimal conditions, TABPT-SPDA-COF shows outstanding enrichment capacity for PPTs in contrast to commercial absorbents ascribed to size selectivity and multiple interaction effects. The method exhibits excellent linear range (0.005-100 ng mL-1), satisfactory limits of detection (0.1 pg mL-1) as well as relative recoveries (86.2-116 %). This work offers a practicable platform to monitor trace PPTs from complex animal-derived foodstuffs.