Effective enrichment and separation of three flavonoids from Ohwia caudata (Thunberg) H. Ohashi using magnetic layered double hydroxide/ZIF-8 composites and pCEC.

In this study, Fe3O4@ZnCr-layered double hydroxide/zeolitic imidazolate frameworks-8 (MLDH/ZIF-8) magnetically functionalized composites were synthesized by co-precipitation and in situ growth based on the advantages of LDHs and ZIF-8 using Fe3O4 nanoparticles as a magnetic substrate to obtain adsorbents with excellent performance. Moreover, the composite was used for the efficient enrichment of flavonoids in Chinese herbal medicines. The internal structures and surface properties were characterized by SEM, Fourier transform infrared spectroscopy, X-ray diffraction and so on. MLDH/ZIF-8 exhibited a large specific surface area and good paramagnetic properties. The MLDH/ZIF-8 magnetic composite was used as a magnetic solid-phase extraction (MSPE) adsorbent, and a MLDH/ZIF-8 MSPE-pressurized capillary electrochromatography coupling method was developed for the separation and detection of flavonoids (luteolin, kaempferol and apigenin) in a sample of the Chinese herb Ohwia caudata (Thunberg) H. Ohashi. The relevant parameters affecting the extraction efficiency were optimized to determine the ideal conditions for MSPE. 5 mg of adsorbent in sample solution at pH 6, vortex extraction for 5 min, elution with 1.5 mL of ethyl acetate for 15 min. The method showed good linearity in the concentration range of 3-50 µg mL-1 with correlation coefficients of 0.9934-0.9981, and displayed a relatively LODs of 0.07-0.09 µg mL-1. The spiked recoveries of all analytes ranged from 84.5% to 122.0% with RSDs (n=3) between 4.5% and 7.7%. This method is straightforward and efficient, with promising potential in the separation and analysis of active ingredients in various Chinese herbal medicines.

A novel sensor based on Ti3C2 MXene/Co3O4/carbon nanofibers composite for the sensitive detection of 4-aminophenol.

A novel, sensitive Ti3C2 MXene/Co3O4/carbon nanofibers (Ti3C2 MXene/Co3O4/CNFs) composite was synthesized via a HF exfoliating Ti3AlC2 strategy, followed by doping Co3O4 and Ti3C2 MXene into the CNFs via a combination electrospinning and thermal annealing process. Ti3C2 MXene/Co3O4/CNFs composite exhibits higher catalytic effect, conductivity, chemical stability, and electrochemical performance than Co3O4 and Ti3C2 MXene in electrochemical impedance, differential pulse stripping voltammetry, chronocoulometry, and cyclic voltammetry tests. This Ti3C2 MXene/Co3O4/CNFs hybrid modified electrode provides fast analysis of 4-aminophenol (4-AP) with ultrahigh sensitivity, enhanced reproducibility and strong anti-interference capability. Furthermore, the level of 4-AP was quantified by this electrode with a wide linear range from 0.5 to 150 µM (R2 > 0.99) and a low detection limit about 0.018 µM was achieved. Finally, the fabricated electrode was used for fast and sensitive analysis of 4-AP spiked in tap water and blood serum samples. This work presents the new Ti3C2 MXene/Co3O4/CNFs electrode provides a platform for 4-AP monitoring and has the advantages of high selectivity, accuracy, simplicity, and rapid analysis.

MoS2 nanosheets grown on bowl-shaped hollow carbon spheres as an efficient electrochemical sensor for ultrasensitive determination of nephrotoxic aristolochic acids in Chinese traditional herbs.

Aristolochic acid, a substance in herbs, is highly nephrotoxic, so it is crucial to develop an assay that can rapidly and accurately analyze its content. In this study, bowl-shaped hollow carbon spheres (BHCs) were synthesized using a complex template method, and a MoS2 layer was grown in situ on their surface using a hydrothermal method. The synthesized MoS2-BHCs were used to fabricate an electrochemical sensor for the ultrasensitive and highly selective detection of aristolochic acids (AAs). The optimal conditions for AA detection were determined by tailoring the amount of MoS2 used to modify the BHCs and the pH of the electrolyte. Under optimal conditions, the MoS2-BHC-based sensor presented excellent AA detection performance. The linear concentration ranges of the MoS2-BHC-based sensor for the detection of AA were 0.05-10 µmol L-1 and 10-80 µmol L-1, and the limit of detection of the sensor was 14.3 nmol L-1. Moreover, the MoS2-BHC-based sensor detected AA in Aristolochia and Asarum sieboldii samples. The results were consistent with high-performance liquid chromatography data, demonstrating the satisfactory recovery and accuracy of the sensor. Therefore, we believe that MoS2-BHC-based sensors can be used as effective platforms for detecting AA in traditional Chinese herbs.

Boron-cluster-based porous BCN material modified electrode for electrochemical determination of morphine in serum.

Porous highly boron-doped BCN (p-BCN) was produced by using a boron cluster salt (closo-[B12H12]2-) as the boron-based precursor and SiO2 as a hard template. The synthesized p-BCN was used in an electrochemical sensor for the ultrasensitive and highly selective detection of morphine (MOP). The optimal conditions for MOP detection were determined by optimizing the experimental conditions. Under these optimal conditions, the p-BCN-based sensor exhibited excellent MOP detection performance (working potential of 0.2 V). Specifically, it showed a detection range of 0.05 to 200 µM and a detection limit of 17.8 nM. Notably, the p-BCN-based electrochemical sensor was successfully applied to the determination of MOP in human blood, and the results showed satisfactory recovery and accuracy. Therefore, this sensor can be used as an effective platform for the detection of MOP in human blood samples.

Rapid quantitative detection of luteolin using an electrochemical sensor based on electrospinning of carbon nanofibers doped with single-walled carbon nanoangles.

In this study, single-walled carbon nanoangles/carbon nanofibers (SWCNHs/CNFs) were synthesized by electrospinning, followed by annealing in a N2 atmosphere. The synthesized composite was structurally characterized by scanning electron microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy. The electrochemical sensor was fabricated by modifying a glassy carbon electrode (GCE) for luteolin detection, and its electrochemical characteristics were investigated using differential pulse voltammetry, cyclic voltammetry, and chronocoulometry. Under optimized conditions, the response range of the electrochemical sensor to luteolin was 0.01-50 µM, and the detection limit was 3.714 nM (S/N = 3). The SWCNHs/CNFs/GCE sensor showed excellent selectivity, repeatability, and reproducibility, thus enabling the development of an economical and practical electrochemical method for the detection of luteolin.

Solid-phase microextraction with MIL-53(Al)-polymer monolithic column coupled to pressurized capillary electrochromatography for determination of chlorogenic acid and ferulic acid in sugarcane samples.

In this paper, a polymer monolithic column based on poly (Butyl methacrylate-co-ethylene glycol dimethacrylate) (poly (BMA-co-EDGMA)) doped with MIL-53(Al) metal-organic framework (MOF) was prepared using an in situ polymerization method. The characteristics of MIL-53(Al)-polymer monolithic column were studied through scanning electron microscopy (SEM), Fourier transform infrared spectrometry (FT-IR), energy-dispersive spectroscopy (EDS), X-ray powder diffractometry (XRD), and nitrogen adsorption experiment. Due to its large surface area, the prepared MIL-53(Al)-polymer monolithic column has good permeability and high extraction efficiency. Using MIL-53(Al)-polymer monolithic column for solid-phase microextraction (SPME), coupled to pressurized capillary electrochromatography (pCEC), a method for the determination of trace chlorogenic acid and ferulic acid in sugarcane was established. Under optimized conditions, chlorogenic acid and ferulic acid have a good linear relationship (r ≥ 0.9965) within the concentration range of 50.0-500 µg/mL, the detection limit is 0.017 µg/mL, and the relative standard deviation (RSD) is less than 3.2%. The spike recoveries of chlorogenic acid and ferulic acid were 96.5% and 96.7%, respectively. The results indicate that the method is sensitive, practical, and convenient. It has been successfully applied to the separation and detection of trace organic phenolic compounds in sugarcane samples.

Electrochemiluminescence Sensor based on Electrospun Crosslinked Carbon Nanofibers for the Detection of Difenidol Hydrochloride.

BACKGROUND: Cross-linked porous carbon nanofibers (CNF) were successfully prepared by electrospinning and high-temperature carbonization. Polyacrylonitrile (PAN) as the carbon source and genipin as the cross-linking agent were used to prepare cross-linked porous carbon nanofibers (CNF). MATERIALS AND METHODS: The field emission scanning electron microscopy (SEM), transmission electron microscope (TEM), automatic specific surface and porosity analyzer Brunner Emmet Teller (BET), X-ray diffraction (XRD), and a laser confocal microspectroscope (Raman, XploRA PLUS, Horiba) were used to characterize the materials. The CNF suspension was dropped on the surface of the bare glassy carbon electrode by the drip coating method to obtain a CNF-modified electrode. Cyclic voltammetry was used to study the electrochemiluminescence behavior of difenidol hydrochloride on CNF-modified glassy carbon electrode (Glassy Carbon Electrode, GCE). RESULTS AND DISCUSSION: Herein, we synthesised a kind of crosslinked carbon nanofibers and designed a novel ECL biosensor. Under the optimal conditions, the concentration of difenidol hydrochloride exhibited a linear relationship with the peak current in the range of 8.0×10-8 to 1.0×10-4 mol/L, with the correlation coefficient of R2=0.997, and a low detection limit (1.2×10-8 mol/L). Difenidol hydrochloride in difenidol hydrochloride tablets was tested, and the recovery rate of sample addition was estimated to be 83.17%-92.17%, and the RSD value to be <5.0%. The designed platform exhibited excellent analytical performance for difenidol hydrochloride determination.

Sensitive and selective electrochemical determination of uric acid in urine based on ultrasmall iron oxide nanoparticles decorated urchin-like nitrogen-doped carbon.

Hypercrosslinked pyrrole was synthesized via the Friedel-Crafts reaction and then carbonized to obtain urchin-like nitrogen-doped carbon (UNC). Ultrasmall iron oxide nanoparticles were then supported on UNC, and the composite was used to prepare an electrochemical sensor for detecting uric acid (UA) in human urine. FexOy/UNC was characterized and analyzed via scanning electron microscopy, transmission electron microscopy, energy dispersive spectrometry, X-ray diffraction, and X-ray photoelectron spectroscopy. A glassy carbon electrode (GCE) modified with FexOy/UNC was used as an electrochemical sensor to effectively identify UA. The electrochemical behavior of the FexOy/UNC-based UA sensor was studied using differential pulse stripping voltammetry, and the optimal conditions were determined by changing the amount of FexOy/UNC, pH of the buffer solution, deposition potential, and deposition time. Under optimal conditions, the FexOy/UNC-based electrochemical sensor detected UA in the range of 2-200 µM, where the limit of detection (LOD) for UA was 0.29 µM. Anti-interference experiments were performed, and the sensor was applied to the actual analysis of human urine samples. Urea, glucose, ascorbic acid, and many cations and anions present at 100-fold concentrations relative to UA did not strongly interfere with the response of the sensor to UA. The FexOy/UNC electrochemical sensor has high sensitivity and selectivity for uric acid in human urine samples and can be used for actual clinical testing of UA in urine.

Determining three isoflavones from Pueraria lobata using magnetic ZIF-8 nanoparticle-based solid-phase extraction and pressurized capillary electrochromatography.

In this study, magnetic functionalized ZIF-8 nanoparticles were prepared by electrostatic self-assembly using magnetic Fe3O4 nanoparticles as cores and ZIF-8 as shells. ZIF-8 was used as the adsorbent to efficiently extract and sensitively analyze isoflavones due to its positive charge and strong adsorption capacity. Prepared samples were investigated by SEM and TEM, BET and ζ-potential analyses, FT-IR spectroscopy, powder XRD, and vibrating sample magnetism (VSM) experiments. The synthesized ZIF-8 has a dodecahedral structure that adsorbs well. Magnetic functionalized ZIF-8/Fe3O4 @SiO2 nanoparticles were prepared as a new SPE adsorbent, and a magnetic ZIF-8-pressurized capillary electrochromatography (pCEC) method was developed to separate and detect puerarin, daidzin, and daidzein (isoflavones) from Pueraria lobata by optimizing the extraction conditions, including adsorbent dosage, salt concentration, extraction time, desorption conditions, and other parameters. The developed method exhibited good linearities in the 50-2000 µg/mL concentration range for the three isoflavones, with coefficients of determination of 0.9934-0.9962. The limits of detection (LODs) for puerarin, daidzin, and daidzein were determined to be 0.02, 0.03, and 0.03 µg/mL, respectively. All analytes showed average recoveries in the 98.5-100.3% range, with relative standard deviations (RSDs, n = 6) of less than 4.0%. The developed method is convenient, enriches effectively, and shows good applications prospects for separating and analyzing components in Chinese herbal medicines.

A facile fabrication of a hierarchical ZIF-8/MWCNT nanocomposite for the sensitive determination of rutin.

In this paper, a novel type of zeolitic imidazolate framework-8 (ZIF-8) polyhedron/multi-walled carbon nanotube (MWCNT) modified electrode was successfully prepared for effective on-site detection of rutin. The morphology and microstructure of the ZIF-8/MWCNT nanocomposite were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The electrochemical performance of the ZIF-8/MWCNT based electrode for the determination of rutin was studied by cyclic voltammetry (CV) and differential pulse stripping voltammetry (DPV). The as-prepared sensor illustrates better electrocatalytic activity and lower background current than the MWCNT modified electrode for the oxidation of rutin. Besides, the ZIF-8/MWCNTs sensor offers a remarkable linear response for rutin concentrations from 0.1 to 15 µM. The detection limit (LOD) was calculated to be 0.26 nM (S/N = 3). Also, the ZIF-8/MWCNT electrode showed high anti-interference ability towards common interfering species. More importantly, the fabricated electrode was quickly evaluated for determination of rutin in medicine tablets with satisfactory recoveries and the obtained results successfully achieved good consistency with the data from high performance liquid chromatography (HPLC). Finally, the method shows an enhanced electrocatalytic property and sensitivity for the analysis of rutin, which may provide an economical and promising electrochemical sensor for practical on-site detection of rutin.

Electrochemiluminescence Sensor Based on Electrospun Three-Dimensional Carbon Nanofibers for the Detection of Difenidol Hydrochloride.

The detection of difenidol hydrochloride, which is a drug that is widely used for treating the nausea and vomiting symptoms caused by certain diseases, has been increasingly involved in cases of suicide via overdosing and of drug poisoning in children. A novel electrochemiluminescence (ECL) sensor for the simple and effective detection of difenidol hydrochloride was fabricated by modifying a glassy carbon electrode with three-dimensional carbon nanofibers (3D-CNFs). The 3D-CNFs were synthesized by electrospinning a mixture of montmorillonite (MMT) and polyacrylonitrile, carbonizing the electrospun product, and etching it with hydrofluoric acid. The form and structure of the 3D-CNFs was analyzed via scanning electron microscopy, X-ray photoelectron spectroscopy, and Raman microspectroscopy. According to the experimental results obtained using the modified electrodes, a good linear relationship was found between peak intensity and difenidol concentration (y = 868.14x - 61.04, R2 = 0.999), with a relatively low detection limit (8.64 × 10-10 mol·L-1 (S/N = 3)). In addition, our approach exhibited good recovery values ranging from 98.99% to 102.28%. The proposed novel ECL sensor has wide application prospects for the detection of difenidol hydrochloride.

Fumigaclavine C attenuates adipogenesis in 3T3-L1 adipocytes and ameliorates lipid accumulation in high-fat diet-induced obese mice.

Fumigaclavine C (FC), an active indole alkaloid, is obtained from endophytic Aspergillus terreus (strain No. FC118) by the root of Rhizophora stylosa (Rhizophoraceae). This study is designed to evaluate whether FC has anti-adipogenic effects in 3T3-L1 adipocytes and whether it ameliorates lipid accumulation in high-fat diet (HFD)-induced obese mice. FC notably increased the levels of glycerol in the culture supernatants and markedly reduced lipid accumulation in 3T3-L1 adipocytes. FC differentially inhibited the expressions of adipogenesis-related genes, including the peroxisome proliferator-activated receptor proteins, CCAAT/enhancer-binding proteins, and sterol regulatory element-binding proteins. FC markedly reduced the expressions of lipid synthesis-related genes, such as the fatty acid binding protein, lipoprotein lipase, and fatty acid synthase. Furthermore, FC significantly increased the expressions of lipolysis-related genes, such as the hormone-sensitive lipase, Aquaporin-7, and adipose triglyceride lipase. In HFD-induced obese mice, intraperitoneal injections of FC decreased both the body weight and visceral adipose tissue weight. FC administration significantly reduced lipid accumulation. Moreover, FC could dose-dependently and differentially regulate the expressions of lipid metabolism-related transcription factors. All these data indicated that FC exhibited anti-obesity effects through modulating adipogenesis and lipolysis.