•PT-SPE method was developed for the enrichment of 16 PAHs in human blood.•The PT-SPE procedure was solvent-saving, reusable, and needed less blood sample.•The method provided referenced information ...for assessing risks of PAH exposure in China.
Polycyclic aromatic hydrocarbons (PAHs) are ubiquitously found in the environment and have been proved to be prospectively associated with the risk of cancer. In this study, a simple method based on pipette-tip solid phase extraction (PT-SPE) and gas chromatography-mass spectrometry (GC–MS) has been firstly developed for the determination of 16 PAHs in human whole blood. Three-dimensional ionic liquid-ferrite functionalized graphene oxide nanocomposite (3D-IL-Fe3O4-GO) was used as sorbent in PT-SPE. Compared with conventional SPE method, the PT-SPE method was solvent-saving (1.0 mL), reusable (at least 10 times) and required less blood sample (200 μL). Affecting parameters on extraction efficiency were investigated and optimized. Under the optimized conditions, a good linearity was obtained and the recoveries of 16 PAHs at three spiked levels ranged from 85.0% to 115%. The limits of quantification (LOQs) were in the range of 0.007-0.013 μg/L. Furthermore, the developed method was successfully applied to the analysis of 16 PAHs in 14 human blood samples. The results showed that the predominant PAHs in human whole blood was low-molecular-weight PAHs, with the rank order phenanthrene (PHE)> naphthalene (NAP)> fluorene (FLU)> fluoranthene (FLT)> pyrene (PYR). Because of its simplicity, accuracy and reliability, the PT-SPE method combined with GC–MS demonstrated the applicability for clinical analysis and provided more information for PAHs exposure studies.
This study aimed to develop a green and efficient approach based on pulsed electric field (PEF) in combination with deep eutectic solvents (DESs) to enhance the antiglycation ability of Noni ...flavonoids (NFs) by modulating their proportions of flavone glycosides and aglycones. The results showed that the proportion of quercetin was elevated with the increasing PEF treatment times at fixed treatment conditions (PEF conditions: 2 kV/cm, 30 μs, 10 Hz; DES: 100% choline chloride/oxalic acid). After 4000 PEF treatments, the molar ratio of rutin and quercetin in the NF sample changed from 0.92:0.08 to 0.09:0.91. Simultaneously, the inhibitory effects of the NF sample treated with 4000 pulses (NF4) on fructosamine, α-dicarbonyl, and advanced glycation end products (AGEs) in the bovine serum albumin (BSA)–fructose model were increased by 2.53, 2.98, and 1.23 times, respectively. This enhancement may be attributed to NF4 exhibiting a greater ability to bind protein and trap methylglyoxal (MGO) compared with untreated samples. Consequently, NF4 can more effectively prevent oxidative damage to the BSA structure, reducing protein aggregation and blocking the accumulation of AGEs. In summary, the combination of PEF with DESs presents a promising and sustainable method to effectively improve the antiglycation ability of Noni flavonoids, showing great potential for the functional food industry.
The novel quaternary ammonium modified magnetic carboxyl-carbon nanotubes (QA-Mag-CCNTs) have been synthesised and characterized. QA-Mag-CCNTs were applied in magnetic dispersive solid phase ...extraction (Mag-dSPE) for preconcentration of perchlorate from tea leaves prior to liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS) analysis. The Mag-dSPE procedure for preconcentration of perchlorate succeed in overcoming the flaw (containing target analyte randomly) of commercially available SPE cartridge. Under optimal conditions, the results showed higher extraction efficiency of QA-Mag-CCNTs, with recoveries between 85.2% and 107%. And the satisfactory precision with inter-day and intra-day RSD values were lower than 8.0%. Furthermore, QA-Mag-CCNTs were evaluated for reuse up to 20 times. The limit of quantification (LOQ) for perchlorate was 8.21 ng kg−1. The developed method was successfully applied in tea leaves for food-safety risk monitoring in Zhejiang province, China. The results showed the concentrations of perchlorate in 229 out of 240 collected samples were in the range of 0.082–988 μg kg−1. It was confirmed that QA-Mag-CCNTs were highly effective materials used for preconcentration of perchlorate.
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•QA-Mag-CCNTs have been synthesised and characterized by SEM, VSM and XPS.•QA-Mag-CCNTs are evaluated in Mag-dSPE for preconcentration of perchlorate from tea leaves.•It succeeds in overcoming the flaw (containing perchlorate randomly) of SPE cartridge.•The Mag-dSPE procedure is environmental friendly and effective to remove matrix.•Mag-dSPE LC-MS/MS method is efficient and promising for food-safety risk monitoring.
A simple and effective method based on the PRiME (process, robustness, improvements, matrix effects, ease of use) pass-through cleanup procedure followed by ultra-high performance liquid ...chromatography-tandem quadrupole mass spectrometry (UHPLC-MS/MS) was developed for analyzing fipronil and its metabolites in seafoods. Matrix effects in seafoods were effectively improved. Validation results demonstrated that this method was suitable for monitoring fipronil residues in seafoods.
Macrophage survival is believed to be a contributing factor in the development of early atherosclerotic lesions. Dysregulated apoptosis of macrophages is involved in the inflammatory process of ...atherogenesis. Apigenin is a flavonoid that possesses various clinically relevant properties such as anti-inflammatory, antiplatelet, and antitumor activities. Here we showed that apigenin attenuated atherogenesis in apo E - / - mice in an in vivo test. In vitro experiments suggested that apigenin induced apoptosis of oxidized low density lipoprotein- (OxLDL-) loaded murine peritoneal macrophages (MPMs). Proteomic analysis showed that apigenin reduced the expression of plasminogen activator inhibitor 2 (PAI-2). PAI-2 has antiapoptotic effects in OxLDL-loaded MPMs. Enhancing PAI-2 expression significantly reduced the proapoptosis effects of apigenin. Molecular docking assay with AutoDock software predicted that residue Ser473 of Akt1 is a potential binding site for apigenin. Lentiviral-mediated overexpression of Akt1 wild type weakened the proapoptosis effect of apigenin in OxLDL-loaded MPMs. Collectively, apigenin executes its anti-atherogenic effects through inducing OxLDL-loaded MPMs apoptosis. The proapoptotic effects of apigenin were at least partly attributed to downregulation of PAI-2 through suppressing phosphorylation of AKT at Ser473.
Bentonite is a kind of natural clay with good exchanging ability. By exchanging its interlamellar cations with various soluble cations, such as quaternary ammonium cations and inorganic metal ions, ...the properties of natural bentonite can be greatly improved. In this study, hexadecyltrimethylammonium bromide （HDTMA）, CaCl2, MgCl2, FeCl3, AlCl3 were used as organic and inorganic pillared materials respectively to produce several kinds of Ca-, Mg-, Fe-, Al-organo pillared bentonites. Sorption of reactive red X-3B on them was studied to determine their potential application as sorbents in wastewater treatment. The results showed that these pillared bentonites had much improved sorption properties, and that the dye solutions＇ pH value had some effect on the performance of these inorgano-organo pillared bentonites. Isotherms of reactive X-3B on these pillared bentonites suggested a Langmuir-type sorption mechanism.
Objective
To identify the underlying mechanisms of the protective effects of Dingxin Recipe (定: 心方, DXR), a Chinese compound prescription that has been used clinically in China for more than 20 ...years, on ischemia/reperfusion (I/R)-induced arrhythmias in rat model.
Methods
A total of 30 rats were randomly divided into three groups: sham group, I/R group, and DXR-pretreated I/R (DXR-I/R) group. Rats in the DXR-DXRI/R group were intragastrically administrated with DXR (12.5 g/kg per day) for consecutive 7 days, while rats I/in the sham and I/R groups were administrated with normal saline. Arrhythmias were introduced by I/R and electrocardiograms (ECG) were recorded. Two-dimensional (2-D) polyacrylamide gel electrophoresis and matrix-matrixassisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) were used to identify assisted differentially expressed proteins. Immunohistochemistry, real-time quantitative polymerase chain reaction (RQ-RQPCR), Western blot, and enzyme-linked immunosorbent assay (ELISA) were performed to analyze proteins PCR), obtained in the above experiments.
Results
DXR significantly reduced the incidence and mean duration of ventricular tachycardia and ventricular fibrillation and dramatically decreased the mortality, as well as arrhythmia score, compared with those of the I/R group. Among successfully identified proteins, prohibitin (PHB) and heart fatty acid binding protein (hFABP) were up-regulated in DXR-pretreated I/R rats compared with those of the I/R rats. In addition, compared with the I/R group, the level of glutathione (GSH) was elevated accompanied by reduced expressions of interleukin-6 (IL-6) and neutrophil infiltration in I/R rats with DXR pretreatment.
Conclusions
DXR could alleviate I/R-induced arrhythmias, which might be related to increased expression of PHB. The enhanced expression of PHB prevented against the depletion of GSH and consequently inhibited apoptosis of cardiomyocytes. Furthermore, up-regulation of PHB might ameliorate I/R-induced cell death and leakage of hFABP by suppressing neutrophil infiltration and IL-6 expressions.
Through cation-exchanging of montmorillonite, mixed hydroxy Fe-Al-pillared montmorillonites with large basal spacing were synthesized. The application of these mixed hydroxy Fe-Al-pillared ...montmorillonites as adsorbents in the areas of environmental protection and pollution control was investigated. Adsorption of Direct Green B, an organic dye, on OH--Fe--, OH--Al--, OH--Fe--Al-- pillared montmorillonites was studied. Results showed that these pillared montmorillonites had much better adsorption properties than traditional Na-organo-montmorillonite. It was also found that pH of the solutions had great effect on the performance of these hydroxy-metal pillared montmorillonites in treating the wastewater containing Direct Green B.
Mixed hydroxy-Al-Fe pillared montmorillonites with large basal spacing were successfully prepared through cation-exchanging of Na+ - montmorillonite with mixed hydroxy-Al and hydroxy-Fe pillaring ...solutions made from hydrolysis of corresponding metal salts, followed by calcination to convert hydroxy-Al and hydroxy-Fe into intercalated polycations. According to XRD analysis, the basal spacing d(001) of pillared products dramatically enlarged from 12.7 A in the Na-montmorillonite to 81 A in the hydroxy-Fe -montmorillonite and 77.5 A in mixed hydroxy-Al-Fe-montmorillonite. The N2 BET surface areas of the pillared montmorillonites also greatly increased to more than 200 m2/g as compared to about 27 m2/g for the Na-montmorillonite. IR analysis of hydroxy-Fe, and mixed hydroxy-Al-Fe pillared montmorillonites revealed a new absorption vibration at 1384 cm(-1) wavelength. XRF elemental analysis data also showed a high content of Fe2O3 in the hydroxy-Fe pillared montmorillonite.
A simple and effective method based on the PRiME (process, robustness, improvements, matrix effects, ease of use) pass-through cleanup procedure followed by ultra-high performance liquid ...chromatography-tandem quadrupole mass spectrometry (UHPLC-MS/MS) was developed for analyzing fipronil and its metabolites in seafoods. Matrix effects in seafoods were effectively improved. Validation results demonstrated that this method was suitable for monitoring fipronil residues in seafoods.
A simple and effective method based on the PRiME pass-through cleanup procedure followed by UHPLC-MS/MS was developed for analyzing fipronil and its metabolites in seafoods.
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