RESUMEN
Expansins (EXPs) are unique plant cell wall proteins with the ability to induce cell wall expansion and play potential roles in xylem development. In the present study, a total of 25 BpEXP genes were identified in Betula platyphylla. Results of bioinformatics analysis described that BpEXP gene family was highly conserved in the process of evolution. All these genes were clustered into four groups, EXPA (Expansin A), EXPB (Expansin B), EXLA (Expansin-like A) and EXLB (Expansin-like B), according to phylogenetic analysis and BpEXPA1 was highly homologous to PttEXP1 and PttEXP2. The results of RT-qPCR showed that BpEXPA1 was expressed higher in stems and preferentially expressed in the first internodes, followed by apical buds and the third internodes, promoter expression analysis with GUS assay demonstrated that it was expressed in developing xylem, suggesting that BpEXPA1 might be involved in the development of the primary stems of birch. Overexpression of BpEXPA1 can promote cortex cell expansion and then enlarge the cortex cell area and layer, however inhibit the secondary cell wall deposition and result in the thinner cell wall and larger lumens of xylem fiber in transgenic plants. This study will provide information for investigating the regulation mechanism of BpEXP family genes and gene resources for birch genetics improvement.
RESUMEN
A high performance liquid chromatography-ultraviolet-visible detector-electrospray ionization-ion trap-time-of-flight-mass spectrometry-total antioxidant capacity determination (HPLC-UVD-ESI-IT-TOF-MS-TACD) new online technique was developed for efficient screening of potential antioxidant active components in Prunus persica flowers (PPF) from 4 origins. Through this online system, 46 compounds were initially identified, while 20 compounds with DPPH binding activity and 21 compounds with FRAP binding activity were detected. The antioxidant activities of 9 compounds obtained from the screening were then validated in DNA oxidative damage protection study. The results showed that this online system can cope well with the complexity of the samples. This also provides technical basis for rapid screening of antioxidant resources of PPF. In short, this study made the chemical composition of PPF more abundant and its potential antioxidant active compounds more explicit, which provided new ideas for the detection and development of natural antioxidants and provided scientific basis for PPF as functional food.
Asunto(s)
Antioxidantes , Daño del ADN , Flores , Prunus persica , Antioxidantes/farmacología , Antioxidantes/química , Antioxidantes/análisis , Flores/química , Daño del ADN/efectos de los fármacos , Prunus persica/química , Cromatografía Líquida de Alta Presión , Espectrometría de Masa por Ionización de Electrospray , Compuestos de Bifenilo/antagonistas & inhibidores , Compuestos de Bifenilo/química , Extractos Vegetales/química , Extractos Vegetales/farmacología , Estrés Oxidativo/efectos de los fármacos , Picratos/antagonistas & inhibidores , Picratos/químicaRESUMEN
Resistivity data has important applications in geophysical exploration, but the impact of electrode offsets on resistivity response characteristics remains unclear. This study aims to explore the influence of horizontal electrode offset angles and vertical offsets caused by topographical variations on the forward modeling of resistivity data. By analyzing experimental models with different measurement arrays, the paper revealed their influence laws on the buried depth of the target body and resistivity resolution. Utilizing tools like ZondRes3D, we conducted 3D resistivity forward modeling and analyzed the results in detail. It is found that horizontal electrode offsets lead to pseudo-anomalies in the apparent resistivity response, which is related to the offset angles and the number of electrodes. Under different conditions, the horizontal electrode offsets exhibit a "gradient variation" pattern. In addition, topographical variations can also cause distortions and offsets in the apparent resistivity curves and the locations of the anomaly response. Specifically, the measuring lines near the edge of the target bodies are more susceptible to these effects. Based on the comprehensive experimental results, we have drawn several conclusions regarding the impact of electrode offsets and topographical variations, including the effects of offset angles on the pseudo-anomalies, the anomalous response laws under different topographic conditions, as well as anomalous situations under specific angles. These findings provide crucial insights for interpreting resistivity data in geophysical exploration and addressing practical engineering problems, and offer guidance for optimizing measuring line layouts and post-processing terrain correction algorithms.
RESUMEN
INTRODUCTION: Traditional and some scientific literature document the antidiabetic effects of the Ziziphi Spinosae Semen (ZSS). However, the bioactive compounds of ZSS responsible for the antidiabetic effects are not well known. OBJECTIVES: This study aimed to investigate the material basis of the antidiabetic effects of ZSS by inhibiting α-amylase. METHODOLOGY: An online analysis platform was established and optimized using an ultra-performance liquid chromatography-photo-diode array-quadrupole-time-of-flight-mass spectrometry-α-amylase-fluorescence detector (UHPLC-PDA-Q-TOF-MS-α-amylase-FLD) system to screen α-amylase inhibitors in ZSS rapidly. The inhibitory effect of these compounds was confirmed by molecular docking screening. and the molecular interactions between α-amylase and active compounds were evaluated, which strongly supported the experimental results. RESULTS: Seventy-eight compounds were identified in the ZSS extract, eleven of which were screened to have significant α-amylase binding activity. CONCLUSION: This study demonstrated the feasibility of using an established platform to screen for effective components in ZSS, providing a practical method for the rapid screening of potential antidiabetic active ingredients in traditional Chinese medicine.
Asunto(s)
Simulación del Acoplamiento Molecular , alfa-Amilasas , alfa-Amilasas/antagonistas & inhibidores , Cromatografía Líquida de Alta Presión/métodos , Ziziphus/química , Hipoglucemiantes/farmacología , Hipoglucemiantes/química , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/farmacología , Inhibidores Enzimáticos/farmacología , Inhibidores Enzimáticos/química , Espectrometría de Masas/métodosRESUMEN
With the gradual progress of research on proton-conducting metal-organic framework (MOFs), it has become a challenging task to find MOF materials that are easy to prepare and have low toxicity, high stability, and splendid proton conductivity. With the abovementioned objectives in mind, we selected the non-toxic organic ligand 2,5-furandicarboxylic acid and the low toxic quadrivalent metals zirconium(IV) or hafnium(IV) as starting materials and successfully obtained 2 three-dimensional porous MOFs, [M6O4(OH)4(FDC)4(OH)4(H2O)4] [M = ZrIV (1) and HfIV (2)], with ultrahigh water stability using a rapid and green synthesis approach. Their proton conductive ability is remarkable, thanks to the large number of Lewis acidic sites contained in their porous frameworks and the abundant H-bonding network, hydroxyl groups, as well as coordination and crystalline water molecules. The positive correlation of their proton conductivity with relative humidity (RH) and the temperature was observed. Notably, their optimized proton conductivities are 2.80 × 10-3 S·cm-1 of 1 and 3.38 × 10-3 S·cm-1 of 2 under 100 °C/98% RH, which are at the forefront of Zr(IV)/Hf(IV) MOFs with prominent proton conductivity. Logically, their framework features, nitrogen/water adsorption/desorption data, and activation energy values are integrated to deduce their proton conductivity and conducting mechanism differences.
RESUMEN
ETHNOPHARMACOLOGICAL RELEVANCE: Gastrodia elata Bl. (GE) is one of the rare Chinese medicinal materials with a long history of medicine and cooking. It consists of a variety of chemical components, including aromatic compounds, organic acids and esters, steroids, saccharides and their glycosides, etc., which has medicinal and edible value, and is widely used in various diseases, such as infantile convulsions, epilepsy, tetanus, headache, dizziness, limb numbness, rheumatism and arthralgia. It is also commonly used in health care products and cosmetics. Thus, its chemical composition and pharmacological activity have attracted more and more attention from the scientific community. AIM: In this review, the processing methods, phytochemistry and pharmacological activities of GE were comprehensively and systematically summarized, which provides a valuable reference for researchers the rational of GE. MATERIALS AND METHODS: A comprehensive search of published literature and classic books from 1958 to 2023 was conducted using online bibliographic databases PubMed, Google Scholar, ACS, Science Direct Database, CNKI and others to identify original research related to GE, its processing methods, active ingredients and pharmacological activities. RESULTS: GE is traditionally used to treat infantile convulsion, epilepsy, tetanus, headache, dizziness, limb numbness, rheumatism and arthralgia. To date, more than 435 chemical constituents were identified from GE including 276 chemical constituents, 72 volatile components and 87 synthetic compounds, which are the primary bioactive compounds. In addition, there are other biological components, such as organic acids and esters, steroids and adenosines. These extracts have nervous system and cardiovascular and cerebrovascular system activities such as sedative-hypnotic, anticonvulsant, antiepileptic, neuron protection and regeneration, analgesia, antidepressant, antihypertensive, antidiabetic, antiplatelet aggregation, anti-inflammatory, etc. CONCLUSION: This review summarizes the processing methods, chemical composition, pharmacological activities, and molecular mechanism of GE over the last 66 years, which provides a valuable reference for researchers to understand its research status and applications.
Asunto(s)
Epilepsia , Gastrodia , Tétanos , Humanos , Etnofarmacología , Fitoterapia , Gastrodia/química , Mareo/tratamiento farmacológico , Hipoestesia/tratamiento farmacológico , Tétanos/tratamiento farmacológico , Epilepsia/tratamiento farmacológico , Anticonvulsivantes/farmacología , Anticonvulsivantes/uso terapéutico , Cefalea/tratamiento farmacológico , Artralgia/tratamiento farmacológico , Fitoquímicos/farmacología , Fitoquímicos/uso terapéutico , Fitoquímicos/química , Extractos Vegetales/farmacologíaRESUMEN
Xiangdan injection (XDI), as a well-known traditional Chinese medicine injection, is of great significance to treat cardiovascular and cerebrovascular diseases. The haptens causing allergic reactions are urged to be detected due to the adverse reaction. In this study, an efficient approach was established to rapidly identify and screen potential haptens in XDI for the first time by combining high performance liquid chromatography-diode array detector-electrospray ionization-ion trap-time of flight-mass spectrometry with human serum albumin-fluorescence detector (HPLC-DAD-ESI-IT-TOF-MS-HSA-FLD). 21 compounds were identified according to their mass spectrum or comparison with reference substances and 8 salvianolic acids in XDI showed interactions with HSA in varying degrees. After that, surface plasmon resonance (SPR) was applied to screen the compounds showing specific affinity with human serum albumin (HSA). Subsequently, active systemic anaphylaxis (ASA) in guinea pigs was carried out to verify the sensitization of active compounds, In the meantime the serum IgE level before and after challenge was measured by the enzyme-linked immunosorbent assay (ELISA). Ultimately, it was tested that salvianolic acid C had a strong sensitization, in addition, lithospermic acid, rosmarinic acid and salvianolic acid B had potential sensitization. This study suggest that the on-line method provides rapid preliminary searching for haptens in XDI, combined with SPR and ASA, offering an efficient, rapid and comprehensive approach to screen haptens.
Asunto(s)
Haptenos , Albúmina Sérica Humana , Animales , Humanos , Cobayas , Cromatografía de Gases y Espectrometría de Masas , Espectrometría de Masas/métodos , Cromatografía Líquida de Alta Presión/métodos , Espectrometría de Masa por Ionización de Electrospray/métodosRESUMEN
In this study, the first ultra-high performance liquid chromatography-photo-diode array-electrospray ionization-quadrupole-time-of-flight-mass spectrometry-lipoxygenase-fluorescence detector (UPLC-PDA-ESI-Q-TOF-MS-LOX-FLD) online system was developed for the identification and evaluation of anti-inflammatory active ingredients in Polygala tenuifolia Willd. Using this system, the UPLC fingerprints, mass fragments and LOX-binding peak profiles in the samples were rapidly and simultaneously obtained. A total of 101 compounds were isolated and identified and 38 compounds (11 oligosaccharide esters, nine xanthones, 17 saponins, and one glycosyloxyflavone) showed strong LOX-binding activity. Six compounds were selected to study their LOX-binding ability, and the results indicated that the content of the six compounds had a good linear relationship with the LOX-binding ability, and it was found that the substitution position, the type of substituent and the number of glycosyl groups all had a certain influence on the LOX-binding ability of the compounds. The LOX-binding activities of 10 compounds were verified by the surface plasmon resonance (SPR) technique and the activity results were consistent with the online system. After validation, we identified 7 active compounds that combined with LOX to exert anti-inflammatory effects for the first time. All the results fully demonstrate the efficiency, stability and reliability of the online system and this work provides an exemplary and useful method for the rapid screening of potential anti-inflammatory active compounds in P. tenuifolia and other traditional Chinese medicines. At the same time, it provides a new direction for screening small molecule inhibitors of enzymes like LOX.
Asunto(s)
Polygala , Saponinas , Polygala/química , Reproducibilidad de los Resultados , Espectrometría de Masa por Ionización de Electrospray/métodos , Medicina Tradicional China , Cromatografía Líquida de Alta Presión/métodosRESUMEN
Amyotrophic lateral sclerosis (ALS) is a progressive neurodegenerative disease affecting both upper and lower motor neurons (MNs) with large unmet medical needs. Multiple pathological mechanisms are considered to contribute to the progression of ALS, including neuronal oxidative stress and mitochondrial dysfunction. Honokiol (HNK) has been reported to exert therapeutic effects in several neurologic disease models including ischemia stroke, Alzheimer's disease and Parkinson's disease. Here we found that honokiol also exhibited protective effects in ALS disease models both in vitro and in vivo. Honokiol improved the viability of NSC-34 motor neuron-like cells that expressed the mutant G93A SOD1 proteins (SOD1-G93A cells for short). Mechanistical studies revealed that honokiol alleviated cellular oxidative stress by enhancing glutathione (GSH) synthesis and activating the nuclear factor erythroid 2-related factor 2 (NRF2)-antioxidant response element (ARE) pathway. Also, honokiol improved both mitochondrial function and morphology via fine-tuning mitochondrial dynamics in SOD1-G93A cells. Importantly, honokiol extended the lifespan of the SOD1-G93A transgenic mice and improved the motor function. The improvement of antioxidant capacity and mitochondrial function was further confirmed in the spinal cord and gastrocnemius muscle in mice. Overall, honokiol showed promising preclinical potential as a multiple target drug for ALS treatment.
RESUMEN
In this study, for the first time, a novel separation and preconcentration method of direct immersion dual-drop microextraction (DIDDME) was proposed for the species of inorganic chromium (Cr(III) and Cr(VI)) followed by graphite furnace atomic absorption spectrometry detection. The methodology is based on that two organic drops hold on the needle tips of microsyringes were concurrently immersed in a stirred sample solution. Each drop contains a chelating reagent, which can react with a specific species under the same pH value. Therefore, Cr(III) and Cr(VI) can be selectively extracted into different drops. This procedure did not require tedious and complicated pre-oxidation/pre-reduction and centrifugation/filtration operations, which may lead to the risk of sample contamination and analysis errors. Main parameters influencing separation, preconcentration and identification of the target species were investigated. An enrichment factor of 400-fold was obtained for Cr(III) and Cr(VI). Under the optimized conditions, detection limits for this method were 1.1 ng L-1 and 1.4 ng L-1 for Cr(III) and Cr(VI) with relative standard deviations of 5.1 and 6.3%, respectively. This procedure was applied for the separation, preconcentration and determination of Cr(III) and Cr(VI) in environmental water samples and certified reference materials with satisfactory results. Recoveries of spiked experiments ranged from 86.0 to 112%.
Asunto(s)
Inmersión , Contaminantes Químicos del Agua , Cromo/química , Quelantes/química , Agua , Concentración de Iones de Hidrógeno , Espectrofotometría Atómica/métodos , Contaminantes Químicos del Agua/análisisRESUMEN
Non-chromatographic speciation methods generally involve speciation conversion, which may cause sample contamination, analysis errors and tedious operations. In this work, a direct immersion dual-drop microextraction (DIDDME) was firstly developed for separation and preconcentration of Cr(III) and Cr(VI). In DIDDME, two organic drops on needle tips of microsyringes were concurrently immersed in a stirred sample solution. Each drop contains a chelating reagent for reacting with a specific species. Thus, Cr(III) and Cr(VI) were selectively extracted into different drops. This method afforded detection limits of 3.0 and 4.1 ng/L, quantification limitof 10 ng/L and 14 ng/L, linear range of 0.01-30 ng mL-1 and enrichment factors of 354-fold and 326-fold for Cr(III) and Cr(VI), respectively. Precisions like repeatability and reproducibility were assessed by calculating relative standard deviations, which were lower than 5.4 % and 6.9 %, respectively. This procedure was used successfully for quantification of Cr(III) and Cr(VI) in food samples.
Asunto(s)
Grafito , Espectrofotometría Atómica/métodos , Inmersión , Reproducibilidad de los Resultados , Cromo/análisisRESUMEN
Targeted high-throughput screening of inhibitors from natural products is an effective approach in the treatment of cancer progression. RhoA protein is essential for many signaling pathways. It is closely related to the occurrence and development of tumor. So far, there are only a few reports on the screening of small molecule inhibitors of RhoA protein from natural products. In this study, an online UHPLC-PDA-MS2-RhoA-FLD screening system was established for the first time to identify RhoA inhibitors from medicinal Alisma. Using this online system by adding fluorescent probes protopine [LZ1] to proteins, 17 active components were identified from Alisma, including 14 terpenoids. Their binding abilities were evaluated by Surface Plasmon Resonance experiments. The activities of representative compounds were tested and showed anti-proliferative effect in cancer cells. Mechanistic studies showed that these compounds were able to downregulate the cellular expressions of RhoA associated proteins. This study provides potential lead compounds as small molecule inhibitors of RhoA protein for cancer therapy. This reported method can be used for targeted screening of small molecule inhibitors against tumors, and provides an approach for screening tumor inhibitors from natural products.
Asunto(s)
Alisma , Productos Biológicos , Proteína de Unión al GTP rhoA/metabolismo , Sistemas en LíneaRESUMEN
To identify natural products as new prototypes for 5-lipoxygenase (5-LOX), 12 traditional Chinese medicines (TCMs) were selected for screening their 5-LOX inhibition activities. The results showed that the methanol extracts of all selected TCMs (n = 12) possessed inhibitory activities against 5-LOX at 200 µg/mL, of which six extracts of the TCMs showed significant inhibitory effects with IC50 values in the range from 33.2 ± 1.4 µg/mL to 153.5 ± 1.7 µg/mL, and the extract of Polygoni Cuspidati Rhizoma (RPC) was the most active sample. An on-line ultra-performance liquid chromatography-photodiode array-MSn -5-LOX-fluorescence detector (UPLC-PDA-MSn -5-LOX-FLD) method was applied to further identify the potential 5-LOX inhibitory constituents in RPC extracts, which resulted in the identification of seven components with 5-LOX-binding activities. Finally, four compounds (polydatin, resveratrol, emodin-8-O-glucoside, and emodin) were successfully purified from RPC extracts. The 5-LOX inhibition action was assayed in vitro, and the results showed that these compounds possessed potent inhibitory effects against 5-LOX with IC50 values of 15.3 ± 2.1, 4.5 ± 1.2, 23.8 ± 0.4, and 11.8 ± 1.5 µg/mL, respectively. This was the first study to reveal the 5-LOX inhibitory constituents of RPC, and the present investigation might provide a valuable approach for the rapid discovery of natural inhibitors from TCMs.
Asunto(s)
Medicamentos Herbarios Chinos , Emodina , China , Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/farmacología , Inhibidores de la Lipooxigenasa/farmacologíaRESUMEN
BACKGROUND: Zika virus (ZIKV) and dengue virus (DENV) cause microcephaly and dengue hemorrhagic fever, respectively, leading to severe problems. No effective antiviral agents are approved against infections of these flaviviruses, calling for the need to develop potent therapeutics. We previously identified gossypol as an effective inhibitor against ZIKV and DENV infections, but this compound is toxic and not suitable for in vivo treatment. RESULTS: In this study, we showed that gossypol derivative ST087010 exhibited potent and broad-spectrum in vitro inhibitory activity against infections of at least ten ZIKV strains isolated from different hosts, time periods, and countries, as well as DENV-1-4 serotypes, and significantly reduced cytotoxicity compared to gossypol. It presented broad-spectrum in vivo protective efficacy, protecting ZIKV-infected Ifnar1-/- mice from lethal challenge, with increased survival and reduced weight loss. Ifnar1-/- mice treated with this gossypol derivative decreased viral titers in various tissues, including the brain and testis, after infection with ZIKV at different human isolates. Moreover, ST087010 potently blocked ZIKV vertical transmission in pregnant Ifnar1-/- mice, preventing ZIKV-caused fetal death, and it was safe for pregnant mice and their pups. It also protected DENV-2-challenged Ifnar1-/- mice against viral replication by reducing the viral titers in the brain, kidney, heart, and sera. CONCLUSIONS: Overall, our data indicate the potential for further development of this gossypol derivative as an effective and safe broad-spectrum therapeutic agent to treat ZIKV and DENV diseases.
Asunto(s)
Virus del Dengue , Dengue , Gosipol , Infección por el Virus Zika , Virus Zika , Animales , Reacciones Cruzadas , Dengue/tratamiento farmacológico , Dengue/prevención & control , Femenino , Gosipol/farmacología , Gosipol/uso terapéutico , Masculino , Ratones , Embarazo , Infección por el Virus Zika/tratamiento farmacológico , Infección por el Virus Zika/prevención & controlRESUMEN
The current non-chromatographic speciation methods generally involve the conversion of different species by oxidation/reduction reactions, which may cause inherent problems such as contamination risk, time consumption and complex operations. In this work, in-syringe solid phase extraction (IS-SPE) was combined with in-syringe vortex-assisted solidified floating organic drop microextraction (IS-VA-SFODME) for the detection of Sb(V) and Sb(III) in rice wines by graphite furnace atomic absorption spectrometry. Firstly, IS-SPE involved the use of ZnFe2O4 nanotubes as the sorbent for the isolation and enrichment of Sb(V) and removal of the matrix components such as ethanol, pigment, sugars and carbohydrates. Then, IS-VA-SFODME was used for enriching Sb(III) in the original sample solution after IS-SPE. This technique exhibited good anti-interference ability and high enrichment efficiency without tedious pre-oxidation/pre-reduction and centrifugation/filtration operations, which may cause the contamination of samples. Under the selected conditions, the detection limits were 4.5 ng L-1 and 3.2 ng L-1 for Sb(III) and Sb(V) with relative standard deviations of 7.3% and 5.1%, respectively. This procedure was used with satisfactory results for the detection of Sb(III) and Sb(V) in rice wine samples and a certified reference material of water sample. Recoveries of spiked experiments ranged from 91.0 to 107%.
Asunto(s)
Grafito , Microextracción en Fase Líquida , Vino , Grafito/química , Microextracción en Fase Líquida/métodos , Extracción en Fase Sólida/métodos , Microextracción en Fase Sólida/métodos , Espectrofotometría Atómica/métodos , JeringasRESUMEN
High-throughput screening of inhibitors from natural products is an efficient approach to target key enzymes in diabetes progression. In this study, an on-line detection system was established for the first time to rapidly screen inhibitors of α-amylase and α-glucosidase from Prunus mume. Among 28 identified compounds, 26 and 21 compounds showed strong inhibitory effect against α-amylase and α-glucosidase, respectively. Their inhibitory effects were validated by in vitro enzyme assay and fluorescence quenching which demonstrated that these inhibitors effectively interfered enzyme active sites. The inhibition kinetics suggested that chemical structures are of great importance for interfering the enzyme structures and their microenvironment polarity. Among evaluated compounds, isorhamnetin-3-O-glucoside (19) showed the strongest binding activities to α-amylase and α-glucosidase (6.34×106·nmol-1 and 6.28×106·nmol-1, respectively) by the on-line detection system. Its IC50 values were 0.16 ± 0.06 and 0.09 ± 0.01 µM against α-amylase and α-glucosidase, respectively. 19 gave a much higher Ki for α-amylase (0.1307 mM) than α-glucosidase (0.0063 mM), indicating its selectivity towards α-glucosidase. This reported method was rapid and reliable to identify prototype inhibitors against key enzymes in diabetes, and thus might serve as a general platform to screen enzyme inhibitors from natural products.
Asunto(s)
Diabetes Mellitus , Prunus , Inhibidores Enzimáticos , Inhibidores de Glicósido Hidrolasas/farmacología , Humanos , alfa-Amilasas , alfa-GlucosidasasRESUMEN
In this work, magnetic dispersive micro-solid phase extraction (MDMSPE) coupled with dispersive liquid-liquid microextraction (DLLME) was developed for Se(IV) and Se(VI) followed by graphite furnace atomic absorption spectrometry. MDMSPE involved the use of magnetic ZnFe2O4 nanotubes for adsorbing Se(VI). The sorbent was isolated from aqueous phase by using an external magnetic field instead of tedious centrifugation or filtration. In the following step, Se(IV) in the upper aqueous phase of MDMSPE was enriched by DLLME. Samples were prepared with artificial gastric juice to avoid the inter-conversion of target species. The main factors affecting the determination of the analytes were studied in detail. the detection limits of this method were 1.0 and 1.3 pg mL-1 for Se(IV) and Se(VI) with relative standard deviations of 4.6% and 5.1% (c = 1.0 ng mL-1, n = 9), respectively. An enrichment factor of 200 was obtained. This method was used for the detection of Se(IV) and Se(VI) in food samples without any pre-oxidation or pre-reduction operation. A certified reference material of milk powder was analysed by this method, and the determined values were in good agreement with the certified values. Recoveries of spike experiments were in the range of 91.0-107%.
Asunto(s)
Análisis de los Alimentos , Contaminación de Alimentos/análisis , Grafito/química , Microextracción en Fase Líquida , Selenio/análisis , Microextracción en Fase Sólida , Fenómenos Magnéticos , Espectrofotometría AtómicaRESUMEN
Magnetic dispersive micro-solid phase extraction (MDMSPE) was coupled with solidified floating organic drop microextraction (SFODME) for direct separation and preconcentration of Mn(II) and Mn(VII) before graphite furnace atomic absorption spectrometry determination. MDMSPE involved use of magnetic ZnFe2O4 nanotubes for adsorbing Mn(VII). Sorbent was isolated from aqueous phase by an external magnet. Mn(II) in upper solution from MDMSPE was further enriched by SFODME. This method avoids tedious pre-oxidation/pre-reduction operation and time-consuming centrifugation/filtration step. An enrichment factor of 200-fold was obtained. Detection limits of this method were 0.005 and 0.007 ng mL-1 for Mn(II) and Mn(VII) with relative standard deviations of 4.0% and 4.8% (n = 9), respectively. This method was successfully used for detection of Mn(II) and Mn(VII) in tap water, ice tea, energy drink, mineral water, sprite drink and carbonated drink. A certified reference material of water sample was analyzed with satisfactory results. Recoveries of spike experiments ranged from 92.5 to 106%.
Asunto(s)
Bebidas/análisis , Manganeso/análisis , Microextracción en Fase Sólida/métodos , Espectrofotometría Atómica/métodos , Grafito/química , Concentración de Iones de Hidrógeno , Solventes/química , Agua/química , Contaminantes Químicos del Agua/análisisRESUMEN
BACKGROUND: Chromium is an interesting element because its toxicity depends on its speciation. Thus, knowledge of Cr speciation in cow milk is essential to human health. OBJECTIVE: This study aims to achieve real bioaccessible species in cow milk, including Cr(III), Cr(VI), residual, digestible, and total Cr. METHODS: Samples were treated with artificial gastric juice, followed by dispersive micro-solid phase extraction (DMSPE) combined with ICP-MS for Cr speciation. Fibrous g-C3N4@TiO2 nanocomposites (FGCTNCs) were used as a novel adsorbent for DMSPE. RESULTS: The method detection limits were 110 pg/g (Cr(III)) and 260 pg/g (Cr(VI)) for milk powder (0.1 g), and 5.1 pg/g (Cr(III)) and 13 pg/g (Cr(VI)) for liquid cow milk (2 mL). The relative standard deviations (RSDs), obtained by analyzing the standard solutions containing 1.0 ng/mL of the analytes in sequence for nine times, were 4.3% and 5.1% for Cr(III) and Cr(VI), respectively. Linearity was observed over the range of 4 magnitude orders with correlation coefficients better than 0.9961. The enrichment factor of 100 was obtained. The majority of Cr in the samples was transferred into digestion solution. The content of Cr(III) is much higher than that of Cr(VI) in the digestion solution. CONCLUSIONS: This method has the advantages of reduced solvent consumption, less adsorbent dosage, and high extraction efficiency. It may become a valuable strategy for elemental species in food samples. HIGHLIGHTS: The samples were treated with artificial gastric juice to avoid the inter-conversion of species. FGCTNCs exhibit the merits of N-rich functional groups and selective adsorption for the analytes.
Asunto(s)
Cromo , Nanocompuestos , Animales , Cromo/análisis , Digestión , Jugo Gástrico/química , Grafito , Humanos , Leche/química , Compuestos de Nitrógeno , Extracción en Fase Sólida , TitanioRESUMEN
An on-line high-performance liquid chromatography-diode-array-detector-electrospray ionization-ion-trap-time-of-flight-mass spectrometry-total antioxidant capacity detection (HPLC-DAD-ESI-IT-TOF-MS-TACD) system was applied for the identification and evaluation of antioxidants in Rosa chinensis Jacq., an edible flower in food industry and a widely used traditional Chinese medicine. With the help of this platform, the HPLC fingerprint, mass fragmentations, and sample activity profiles against 1,1-diphenylpicryl-2-hydrazyl radical (DPPHâ¢) and ferric reducing antioxidant power (FRAP) were recorded after one injection. Using this technique, 80 compounds were separated and identified by their LC/MS behaviors with the assistance of standard compounds. In addition, 11 different Rosa chinensis Jacq. samples were profiled and then quantified for their DPPH⢠and FRAP activities. Interestingly, a total of 52 compounds showed antioxidative effects against DPPH⢠and 61 were active against FRAP. The results demonstrated that the on-line system is a powerful technique for antioxidant discovery in Rosa chinensis Jacq. and other food resources.