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Biomass pelletization technology has recently gained significant interest, where pyrolyzed pellets have a very wide range of applications (e.g., as pellet fuels and adsorbents). In this study, furfural residue pellets (FRPs) were pyrolyzed at temperatures of 200–850 °C in a tube furnace. The physical and chemical properties of the pyrolyzed FRPs (PFRPs) obtained at various temperatures were compared, and the kinetic parameters of the pyrolysis process were calculated using the distributed activation energy model (DAEM). The PFRPs prepared at 450, 650, and 850 °C had higher volumetric energy densities than coal, whereas other properties (e.g., H/C and O/C ratios) were found to be similar to those of coal. The maximum iodine adsorption value (i.e. 317.8 mg/g) and methylene blue adsorption value (i.e. 96.4 mg/g) were achieved by pyrolysis at 650 °C and 450 °C, respectively, indicating that pyrolysis promoted the formation of micropore structures at 650 °C. Two-dimensional correlation spectroscopy (2D-COS) was employed to explore the temperature-sensitivity of the surface functional groups of the PFRPs. Based on comparison of the volumetric energy density, hydrophobicity, particle density, and strength, the PFRPs prepared at 250–300 °C afforded the best overall performance, where the sample prepared at 300 °C exhibited the maximum hydrophobicity.

Activated carbon (AC) was prepared from furfural residue (FR) in a horizontal tube reactor under a carbon dioxide atmosphere comparing one- and two-step activation methods. Considerable differences were observed between ACs produced from these two methods in microscopic morphology, structural properties, organic structure, and crystallinity. It showed that the AC obtained by one-step activation (800 oC, 20 min, K2CO3: FR = 0.5:1) exhibited microporous and alkaline surface characteristics, and achieved the highest iodine value of 1305.7 mg/g and BET surface area 2083.6 m2/g. While, for the two-step method, the iodine value was 1004.9 mg/g and the BET surface area was only 726.3 m2/g. Furthermore, one-step activation obtained a higher yield of high-quality AC in a shorter activation time than the two-step method. The adsorption data fitted well with the Redlich-Peterson isotherm model and reached the highest value of 1761.1 mg/g, while the adsorption kinetics agreed well with the pseudo-second-order model.

Four new polyacetylene substances, sadivaethynes A–D, were isolated from the ethanol extract of the roots of Saposhnikovia divaricata (Turcz.) Schischk using repeated column chromatography. Structu...

A novel compound, 3,7-dichloro-N-(2,6-diethylphenyl)-N-(2-propoxyethyl)quinoline-8-carboxamide was synthesized by splicing together a chloro-substituted quinoline moiety found in quinclorac (a selective herbicide) and a substituted amide moiety found in pretilachlor (another selective herbicide) using the active substructure splicing method. The chemical structure of this compound was characterized by 1H, 13C NMR, FTIR, high-resolution mass spectra and X-ray diffraction analysis. Pesticide potency (herbicidal and fungicidal activity) of this compound was evaluated. This compound displayed excellent control efficiency against Echinochloa crusgalli and also showed good fungicidal in vitro activity against Phytophthora capsici, Phytophthora sojae, and Phytophthora infestans.

There is increasing awareness that oxidative stress may be implicated in the pathophysiology of autism spectrum disorder (ASD). Here we aimed to investigate blood oxidative stress marker profile in ASD children by a meta-analysis. Two independent investigators systematically searched Web of Science, PubMed, and Cochrane Library and extracted data from 87 studies with 4928 ASD children and 4181 healthy control (HC) children. The meta-analysis showed that blood concentrations of oxidative glutathione (GSSG), malondialdehyde, homocysteine, S-adenosylhomocysteine, nitric oxide, and copper were higher in children with ASD than that of HC children. In contrast, blood reduced glutathione (GSH), total glutathione (tGSH), GSH/GSSG, tGSH/GSSG, methionine, cysteine, vitamin B9, vitamin D, vitamin B12, vitamin E, S-adenosylmethionine/S-adenosylhomocysteine, and calcium concentrations were significantly reduced in children with ASD relative to HC children. However, there were no significance differences between ASD children and HC children for the other 17 potential markers. Heterogeneities among studies were found for most markers, and meta-regressions indicated that age and publication year may influence the meta-analysis results. These results therefore clarified blood oxidative stress profile in children with ASD, strengthening clinical evidence of increased oxidative stress implicating in pathogenesis of ASD. Additionally, given the consistent and large effective size, glutathione metabolism biomarkers have the potential to inform early diagnosis of ASD.

Torrefaction integrated with pelletization has gained increasingly interest as it enhances the characteristics of fuel pellets (e.g. hydrophobicity and energy density). In current study, torrefaction of furfural residue pellets (FRPs) and sawdust pellets (SPs) was performed by employing tubular reactor furnace, and quality of pellets was compared. The characteristics of both types of pellets were significantly improved with increasing torrefaction temperature from 200 °C to 300 °C and residence time from 15 min to 30 min. The highest lower heating value of 23.78 MJ/kg and energy density ratio (1.27) for torrefied furfural residue pellets (TFRPs) and 26.76 MJ/kg and 1.46 for torrefied sawdust pellets (TSPs) were achieved at 300 °C and 120 min. Increasing torrefaction temperature and residence time, the volumetric energy densities of TFRPs increased from 25.69 (at 200 °C and 15 min) to 27.59 kJ/m3 (at 300 °C and 120 min), while those of TSPs correspondingly decreased from 20.81 to 16.69 kJ/m3. The highest true densities (i.e. 2.40 and 1.85 g/cm3) and porosities (i.e. 52 and 65 v %) of TFRPs and TSPs were achieved at 300 °C and 120 min, much higher than those of un-torrefied pellets. Moisture uptake of TFRPs and TSPs at 300 °C were only 1.4 wt% and 2.0–2.8 wt%, respectively, showing strong water-resistant ability. The crystallinity of cellulose in FRPs was found higher than that of SPs, while the crystallinity of cellulose in TFRPs was found lower than that of TSPs at same process conditions. FTIR showed that O-H bond was destroyed after torrefaction for both FRP and SP.

Microwave-assisted pyrolysis (MWAP) of furfural residue (FR) was performed in a continuously operated auger reactor. The effects of temperature and additives on pyrolysis products and char properties were investigated. The yield of FRBC (furfural residue biochar) decreased to 43.62 wt.% and non-condensable gas yield increased to 40.37 wt.% with temperature increasing to 750 °C. However, condensate yield increased with increasing temperature from 450 to 550 °C, reaching maximum (i.e. 21.49 wt.%) at 550 °C, then decreased to 15.65 wt.% as temperature reached 750 °C. Kaolin and K2CO3 promoted production of non-condensable gases and CaO increased the yield of FRBC. The relative proportion (RP) values of carbon, hydrogen, nitrogen and sulfur in FRBC were 50.49–65.07 wt.%, 13.05–26.81 wt.%, 61.99–79.84 wt.% and 60.93–74.16 wt.%, respectively. The highest iodine adsorption value of 127mg/g and methylene blue number of 59 mg/g were achieved for FRBC at 450 °C. Kaolin, CaO and K2CO3 increased methylene blue number, and K2CO3 significantly increased iodine adsorption capacity of FRBC. CaO retained sulfur, chlorine, zinc, and kaolin showed greater retention capacities for copper, nickel, chromium and zinc. The major crystalline phases of sulfur and nitrogen were CaSO4, K2Ca2(SO4)3, Zr(NO3)4 in FRBC and K2Ca2(SO4)3 in FR.

Congenital disorders of glycosylation (CDGs) are inherited metabolic diseases affecting protein and lipid glycosylation. DDOST-CDG is a rare, newly identified type of CDGs, with only one case reported so far. In this study, we report a Chinese patient with a homozygous pathogenic variant in DDOST (c.1187G>A) and who presented with feeding difficulty, lactose intolerance, facial dysmorphism, failure to thrive, strabismus, high myopia, astigmatism, hypotonia, developmental delay and situs inversus totalis. Serum transferrin isoelectrofocusing demonstrated defective glycosylation in our patient. This finding further identifies DDOST as a genetic cause of CDGs and expands the clinical phenotype of DDOST-CDG.

Background: The molybdenum cofactor (Moco) deficiency in humans results in the inactivity of molybdenum-dependent enzymes and is caused by pathogenic variants in MOCS1 (Molybdenum cofactor synthesis 1), MOCS2 (Molybdenum cofactor synthesis 2), and GPHN (Gephyrin). These genes along with MOCS3 (Molybdenum cofactor synthesis 3) are involved in Moco biosynthesis and providing cofactors to Moco-dependent enzymes. Until now, there was no study to confirm that MOCS3 is a causative gene of Moco deficiency.Methods: Detailed clinical information was collected in the pedigree. The Whole-exome sequencing (WES) accompanied with Sanger sequencing validation were performed.Results: We described the clinical presentations of an infant, born to a non-consanguineous healthy family, diagnosed as having MOCS3 variants caused Moco deficiency and showing typical features of Moco deficiency including severe neurologic symptoms and cystic encephalomalacia in the brain MRI, resulting in neonatal death. Compound heterozygous variants in the MOCS3 gene were identified by WES. Positive sulfite and decreased levels of uric acid in plasma and urine were detected.Conclusion: To our knowledge, this is the first case of MOCS3 variants causing Moco deficiency. Our study may contribute to genetic diagnosis of Moco deficiency and future genetic counseling.

BACKGROUND The diamondback moth (Plutella xylostella) is one of the most destructive lepidopteran pests on cruciferous vegetables. However, resistance has emerged to current chemical and biological insecticides used for P. xylostella control, indicating the necessity of screening new targets on P. xylostella, and finding new insecticides against P. xylostella. In particular, octopamine receptors are representative G protein-coupled receptors found only in invertebrates and are potential targets for identifying novel insecticides. RESULTS A β-adrenergic-like octopamine receptor gene (PxOA2B1) was cloned, and its pharmacological characteristics in P. xylostella were studied. The results demonstrated that octopamine could activate the PxOA2B1 receptor, with a half-maximal effective concentration (EC50 ) of 49.5 nm. Amitraz, an insecticide and acaricide, and its metabolite (N-2,4-dimethylphenyl-N'-methylformamidine; DPMF) were also found to act as PxOAB1R agonists. We synthesized phenyl imidazolidin-2-one derivatives 3a-h using DPMF as the lead compound, and compounds 3a-h showed similar antagonist activities as phentolamine, mianserin and chlorpromazine. In particular, 3d, with an EC50 of 25.2 nm, showed very similar antagonist activity to mianserin. CONCLUSION This research found that PxOAB1R might be a potential target for P. xylostella control. Phenyl imidazolidin-2-ones could be novel potential antagonists targeted at octopamine receptors and would be useful tools for the design and development of novel insecticides. © 2021 Society of Chemical Industry.

Two new (1-2) and three known quinic acid derivatives (3-5) were isolated from the leaves of Schisandra chinensis (Turcz) Baill. The structures of the compounds were determined by spectroscopic methods, especially the NMR techniques, and also by comparison with reported data in the literature. The cytotoxicity activities of these compounds were evaluated on human tumor cell lines LN229 and three of them showed a certain activity.

Background Microglia-mediated neuroinflammation is associated with epilepsy. Switching microglial polarization from the pro-inflammatory M1 phenotype to the anti-inflammatory M2 phenotype represents a novel therapeutic strategy for mitigating epileptogenesis. We previously found that dynorphins protected against epilepsy via activation of kappa opioid receptor (KOR). Here, this study aims to investigate the role and the mechanism of dynorphin in regulating microglial polarization. Methods A pilocarpine-induced rat model of epilepsy was established and lipopolysaccharide (LPS)-activated BV-2 microglial cells were used as an inflammatory model to explore the mechanism of dynorphin regulating microglial polarization. Results Overexpression of the dynorphin precursor protein prodynorphin (PDYN) alleviated the pilocarpine-induced neuronal apoptosis, promoted microglial polarization to the M2 phenotype, and inhibited pilocarpine-induced Toll-like receptor 4 (TLR4)/nuclear factor-kappa B (NF-κB) pathway in the hippocampi of epileptic rats. Dynorphin activation of KOR promoted microglial M2 polarization via inhibiting TLR4/NF-κB pathway in LPS-stimulated BV-2 microglial cells. Moreover, dynorphin/KOR regulated microglial M2 polarization inhibited apoptosis of the primary mouse hippocampal neurons. Conclusion In conclusion, dynorphin activation of KOR promotes microglia polarization toward M2 phenotype via inhibiting TLR4/NF-κB pathway.

Eight new sesquiterpenoids named melongenaterpenes M-T (1-8), together with nine known compounds (9-17), were isolated from the 70% ethanol extract of the sepals of Solanum melongena L. The structures of all isolated compounds were elucidated based on 1D and 2D NMR spectra and a comprehensive comparison of their spectroscopic and physical data with values from the published literatures. Meanwhile, the cytotoxicity of all the isolated compounds was evaluated on the three human cancer lines of Hela, Ishikawa and MGC-803 by CCK8 assay, respectively.

Fifteen constituents, including one new lignan (schisandroside E) and one new terpenoid (schisandenoid A) as well as nine known lignans and four known terpenoids, were isolated from Schisandra chinensis leaves. The structures of schisandroside E and schisandenoid A were established by entirely meticulous spectroscopic analysis (NMR, MS, CD, IR and UV). All compounds were tested for cytotoxicity against MGC-803, Caco-2 and Ishikawa cell lines. Some compounds showed strong cytotoxicity against these three cancer cell lines with IC50

Two new alkaloids named Melongenamides H-I (1–2), together with twenty-one known compounds (3–23), were isolated from the 70% ethanol extract of the sepals of Solanum melongena L. The structures of all isolated compounds were determined by 1D and 2D NMR spectra and by comparing their spectroscopic and physical data with values from the published literatures. All the isolated compounds were evaluated the cytotoxicity against three human canner lines (Hela, Ishikawa and MGC-803) by CCK8 assay.

A hybrid material of metal organic frameworks (MOFs) and monoliths was developed and used for stir bar sorption extraction (SBSE) of five sulfonylurea herbicides. It was prepared in a glass tube (4 mm I.D.) by thermal polymerization using modified neodymium supermagnetic (Nd2Fe14B) powders as the component substrates, the organic polymerization solutions and ethyl cellulose as the adhesion agent. The prepared stir bar was characterized by scanning electron micrography (SEM) and X-ray diffraction (XRD). It was successfully applied for the determination of sulfonylurea herbicides in soil and lake water samples coupled with high-performance liquid chromatography (HPLC). The extraction and desorption factors affecting the performance of sulfonylurea herbicides were evaluated in detail. Under the optimum conditions, the extraction efficiency of the hybrid stir bar was obviously higher than the blank stir bar without UIO-66(Zr)-NH2. Linear ranges were 10–700 μg/L for thifensulfuron-methyl (TIM), amidosulfuron (AS) and metsulfuron-methyl (MSM) and 10–800 μg/L for sulfosulfuron (SSF) and tribenuron-methyl (TBM), respectively. The obtained detection limits were in the ranges of 0.04–0.84 μg/L with the recoveries of 68.8–98.1% for the real samples. The novel stir bar possessed excellent advantages of both supermagnetic performance and large specific surface areas in the presence of MOFs and monoliths, which was potentially an optimal adsorbent for environmental analysis.

In this study, pelletization of sewage sludge (SS), furfural residue (FR) and corn stalk (CS) and mixture of SS with FR and CS was performed, and various quality parameters and their dependency on process variables were investigated. Addition of SS in ratios of 20–40% to FR had not enhanced the pellet densities (e.g. particle and relaxed) of furfural residue sludge mixed pellets (FRSPs). However, mixing SS with CS in ratio of 20–80% had resulted in higher density, strength and hardness of corn stalk sludge mixed pellets (CSSPs). Addition of sludge to 20% with FR had resulted in higher strength and hardness (i.e. 7 ± 0.22 MPa and 508 ± 28.1 N/mm2) of pellets. While the highest strength and hardness i.e. 13.4 ± 0.12 MPa and 392 ± 5.96 N/mm2 were found for CSSPs-40 and CSSPs-80. Pelletization at 200 °C was found to be beneficial as it improved the mechanical characteristics of FRSPs and CSSPs and reduced the energy consumption. Energy consumption of pellets was decreased markedly with increasing sludge ratio and the lowest was found at SS proportion of 80%. Heating values of sludge mixed pellets were found higher than sewage sludge pellets. Compression models had well evaluated the compaction behavior of FR, SS, CS and their corresponding mixture with R2 ≥ 0.9. Using SS in lower proportion (e.g. 20%) could reduce the odor during pelletization or even in the pellets. The results showed that co-pelletization of SS with FR and CS could be feasible approach to enhance the characteristics of pellets and reduced the energy consumption.

Textile dyeing sludge (DS) was pyrolysed using an auger pyrolyser under microwave irradiation. It showed the non-condensable gas yield was increased as reactor temperature increased and the char yield decreased with temperature. The condensate and oil yields reached maximum at 650 °C (i.e. 12.86 wt% and 0.84 wt%, respectively). The content of C, H and N in DS and sludge char (SC) decreased with temperature while S increased. The SC and sorbents (e.g. CaO) showed positive effects on sulfur retention. The maximum BET surface area of 91.9 m 2 /g was observed for SC at 550 °C. Addition of catalysts such as CaO and Fe decreased pyrolysis oil yield and increased the H 2 yield. Oxygenates were mainly formed at 450–650 °C. The relative content of aromatic compounds in the pyrolysis oil increased as temperature increased, up to 88.38% (GC–MS area) at 750 °C. Heterocyclic aromatic compounds containing nitrogen accounted for 20%–58% of the pyrolysis oil. The H 2 content increased from 25.39 vol% without catalyst to 64.17 vol% with addition of 30 wt% CaO. As concentration in DS and SC was beyond the control standards for forestland use in China and should be further treated and disposed. The electricity consumption for pyrolysing DS of 60 wt% water content were 0.76–2.59 kWh/kg wet DS in the temperature range of 450–750 °C and auger speed range of 1–9 rpm. Higher pyrolysis temperature and lower auger speeds increased electricity consumptions.

This paper investigated an auger pyrolyser under microwave irradiation using textile dyeing sludge (DS) as the feedstock. Microwave power, temperature, auger speed, gas velocity and addition of catalysts were studied. In terms of ICP-MS, Cu and As concentrations in condensates, depending on pyrolysis temperatures, exceeded the wastewater discharge standard in China. The condensate and oil yields reached maximum (i.e. 12.86 wt% and 0.84 wt%, respectively) at 650 °C. The content of aromatic compounds in the oil increased as temperature increased, up to 88.38% (GC-MS area) at 750 °C. Heterocyclic aromatic compounds containing nitrogen accounted for 20%-58% of the pyrolysis oil. Addition of catalysts such as CaO and Fe decreased pyrolysis oil yield and increased the content of H2. The H2 content increased from 25.39v% without catalyst to 64.17v% with addition of 30 wt% CaO. The electricity consumption was 0.80-2.64 kWh/kg wet sludge from 450 to 750 °C and auger speed range of 1-9 rpm. Higher auger speeds and lower temperatures led to lower electricity consumption.

This paper investigated an auger pyrolyser under microwave (MW) irradiation for pyrolysis of textile dyeing sludge (DS). It showed that the sludge char (SC) yield decreased and the yield of non-condensable gas gradually increased with pyrolysis temperature. The condensate and oil yields reached maximum (i.e. 12.9 wt% and 0.8 wt%, respectively) at 650 °C. Addition of CaO and Fe increased the SC yield and H 2 contents, and decreased CO 2 content in the non-condensable gas. The H 2 content increased from 25.4 v% without additives to 64.2 v% with addition of 30 wt% CaO at 650 °C. Whereas Ca-bentonite and kaolin decreased H 2 contents with the latter decreasing SC yields and increasing condensate yields. The content of C, H and N in SC decreased with temperature while S increased. CaO and Ca-bentonite were beneficial for sulfur retention and some heavy metal immobilization for microwave pyrolysis of DS. The maximum BET surface area of 123 m 2 /g was observed for SC with addition of 20 wt% kaolin, consistent with SEM observations. The main components of the pyrolysis oil were analyzed by GC–MS. High proportions of aromatic compounds were found in the pyrolysis oil from different pyrolysis temperatures. Oxygenates were mainly formed in the temperature range of 350–650 °C. The content of aromatic compounds in the oil increased as temperature increased, up to 88.4% (GC–MS area) at 750 °C. Heterocyclic aromatic compounds containing nitrogen accounted for 30% ∼ 50% of the pyrolysis oil. CaO, Fe, Ca-bentonite considerably reduced the aromatics content in the pyrolysis oil. The additives used in this study acted as microwave absorbers (MWAs), catalysts, sorbents and reactants in the microwave assisted pyrolysis of DS. The combined functions of these additives and unique characteristics of MW heating contributed to different product yields, and various product compositions and product properties.

Exosomal microRNAs (miRNAs) have been suggested to participate in the pathogenesis of neuropsychiatric diseases, but their role in major depressive disorder (MDD) is unknown. We performed a genome-wide miRNA expression profiling of blood-derived exosomes from MDD patients and control subjects and revealed the top differentially expressed exosomal miRNA, i.e. hsa-miR-139-5p (upregulation), had good performance to differentiate between MDD patients and controls. Tail vein injection of blood exosomes isolated from MDD patients into normal mice caused their depressive-like behaviors as determined by the forced swimming, tail suspension, and novelty suppressed feeding tests, and injection of blood exosomes isolated from healthy volunteers into unpredictable mild stress (CUMS)-treated mice alleviated their depressive-like behaviors. CUMS mice also showed significantly increased blood and brain levels of exosomal miR-139-5p. Furthermore, the depressive-like behaviors in CUMS-treated mice were rescued by intranasal injection of miR-139-5p antagomir, suggesting that increased exosomal miR-139-5p levels may mediate stress-induced depression-like behavior in mice. Both exosome treatment and miR-139-5p antagomir treatment increased hippocampal neurogenesis in the CUMS-treated mice, and treatment of exosome from MDD patients decreased hippocampal neurogenesis in the normal mice. The role of miR-139-5p in neurogenesis was validated by in vitro experiments, demonstrating that miR-139-5p is a negative regulator for neural stem cell proliferation and neuronal differentiation. Our findings together suggest that exosomes from patients with major depression caused depressive-like behaviors in mice with involvement of miR-139-5p-regulated neurogenesis. Therefore, exosomal miRNAs are promising targets for the diagnosis and treatment of MDD.

Kidney-yin deficiency syndrome (KYDS) is a typical syndrome encountered in traditional Chinese medicine (TCM) and is characterized by impaired lipid and glucose homeostasis. The hypothalamus acts as an important regulatory organ by controlling lipid and glucose metabolism in the body. Therefore, proteins in the hypothalamus could play important roles in KYDS development; however, the mechanisms responsible for KYDS remain unclear. Herein, iTRAQ-based proteomics was performed to analyze the protein expression in the hypothalamus of KYDS rats induced by levothyroxine (L-T4). Results revealed a total of 44 downregulated and 18 upregulated proteins in KYDS group relative to the control group. Gene Ontology (GO) analysis revealed that the differently expressed proteins (DEPs) were related to single-organism metabolism process under the biological process (BP), extracellular region part and organelle under the cellular component (CC), and oxidoreductase activity under the molecular function (MF). Kyoto Encyclopedia of Gene and Genomes (KEGG) analysis showed that fatty acid degradation and pyruvate metabolism participated in the metabolism regulation in KYDS rats. RT-PCR validation of five distinctly expressed proteins related to the two pathways was consistent with the results of proteomics analysis. Taken together, the inhibition of fatty acid degradation and pyruvate metabolism in hypothalamus could potentially cause the dysfunction of the lipid and glucose metabolism in KYDS rats. This current study identified some novel potential biomarkers of KYDS and provided the basis for further research of KYDS.

A single pellet press was employed for production of furfural residue pellets (FRPs) and wood pellets (WPs). The effects of temperature (70–200 °C), pressure (70–160 MPa), moisture content (MC) (5.5–28%), particle size (0.25–0.5 and 0.5–1.41 mm) and a binder on the physical and mechanical characteristics and energy consumption of FRPs and WPs were investigated. Temperature and pressure were found to be the most dominant factors followed by MC and particle size. For FRPs, pellet density, strength and hardness increased with increasing temperature from 70 to 130 °C and increasing pressure from 70 to 160 MPa and then decreased at >130 °C and a MC of 5.5%. The highest particle density of ~1.43 g cm−3, strength >8 and 5.56 MPa, hardness 438.5 and 350.2 N mm−2 for particles 0.25–0.5 and 0.5–1.41 mm, respectively, was found at 130 °C, 160 MPa and 5.5% MC. For WPs, the highest pellet density, strength and hardness were achieved at 200 °C, ≥100 MPa. FRPs and WPs remained dimensionally stable particularly at temperature ≥130 °C, pressure 160 MPa and 5.5% MC. For a MC of 5.5%, pellets made at 200 °C were found to be water resistive. Increasing temperature, MC and use of a binder reduced the energy consumption of FRPs and WPs. Use of a binder was more beneficial for WPs compared to FRPs. FRPs had better quality and lower energy consumption than WPs. Temperatures of 130 °C and 200 °C, particle size of 0.25–0.5 mm and MC of 5.5% and 18% were found to be optimal for FRPs and WPs quality.

Activated carbons (ACs) were prepared from furfural residues (FRs) by microwave-assisted pyrolysis and activation under CO2 atmosphere in this study. At microwave activation temperature of 800 °C and activation time of 20 min, KOH impregnated ACs (MKFRAC*) reached the maximum adsorption ability. While water-washed FRs (MWFRAC*) needed higher processing temperature and longer treatment time (850 °C/60 min) to attain its maximum adsorption capacity. Raman showed MKFRAC* had a high R-value, indicating the graphite structure's low crystallinity caused by the porous structure. The iodine adsorption value, Methylene Blue (MB) number, and yield of MKFRAC* were 1159.1 mg/g, 448.0 mg/g and 26.8% wt%, respectively. The mesopore volume of MKFRAC* was >48%, more than those of other ACs mainly due to the synergistic effect of chemical reagents, carbon structure and microwave irradiation. The investigation on the adsorption mechanism of MB on ACs revealed that MB adsorption capacities of MKFRAC were well described by the Langmuir model, showing a maximum monolayer adsorption capacity of 562.9 mg/g, while MB adsorption kinetics of MKFRAC followed a pseudo-second-order model. The results showed microwave preparation of FR-based ACs was a feasible technique with potential industrial applications.

Microwave-assisted pyrolysis (MAP) of waste printed circuit boards (WPCB) was performed to investigate the characteristics of pyrolysis product and Br fixation. Pyrolysis conversion increased with increasing temperature, reaching 93.3 % at 650 °C. However, increasing heating time did not exhibit remarkable influence on pyrolysis conversion. At 350 °C, phenols were main compounds in the oil accounting for 91.15 %. As the temperature increased to 650 °C, polycyclic aromatic hydrocarbons and monocyclic aromatic hydrocarbons (except phenols) increased to 20.55 % and 19.03 %, respectively. Meanwhile, the total content of CO2, CO, CH4 and H2 in the non-condensable gases increased significantly. Addition of ZSM-5 and kaolin promoted the recombination reaction of pyrolysis products, increased the relative percentage of monocyclic aromatic hydrocarbons (except phenols) and C11-C20 compounds in the oil, and reduced non-condensable gases. The oxygen bomb-ion chromatography was used to evaluate the Br content of pyrolysis residues. Higher pyrolysis temperature enhanced transfer of Br to pyrolysis gas. K2CO3, Na2CO3 and NaOH reacted with hydrogen bromide to generate KBr and NaBr, which significantly improved the Br fixation efficiency of pyrolysis residues (i.e. from 29.11%-99.80%, 96.39 % and 86.69 %, respectively) and reduced Br content in pyrolysis gas.

Using 3-(4-cyano phenoxy)-6-methyl-4-(3-trifluoromethylphenyl) pyridazine (compound ) as a leading compound, a total of 24 novel 3-(substituted phenoxy)-6-methyl-4-(3-trifluoromethylphenyl) pyridazine derivatives containing two electron-withdrawing groups on the benzene ring (acylamine and oxime ether) were synthesized. Their herbicidal, insecticidal activities were bioassayed, and the herbicidal activity of compound against Brassica campestris was 97.6% at 300 g/ha, which was better than the commercial herbicide diflufenican at the this concentration and is equal to the activity of the leading compound . Compound , , , and displayed excellent insecticidal activity against Aphis laburni Kaltenbach (>95%). The results show that the oxime ether substitutions exhibit better bleaching and herbicidal activity than the acylamine ones. The bleaching and herbicidal activity of para-position substitutions is better than the meta-position ones. It seems that the para-position on the benzene ring of oxime ether pyridazine derivatives is one of the key active sites that affect their herbicidal activities.

A highly enantioselective palladium-catalyzed [3 + 2] cycloaddition of propargylic esters with β-ketoesters has been realized by employing a newly developed chiral ferrocene/benzimidazole-based P,N-ligand. This protocol features a good tolerance of functional groups in both propargylic esters and β-ketoesters, thereby delivering a variety of highly functionalized chiral 2,3-dihydrofurans bearing an exocyclic double bond at the 3-position in good yields and with high enantioselectivities (up to 98% ee).

This paper investigated fluidized bed pyrolysis (FBP) and microwave-assisted auger pyrolysis (MWAP) for treatment and disposal of textile dyeing sludge (DS), and the products were analyzed and compared. MWAP achieved higher yields of char and condensate, and lower non-condensable gas yields compared to FBP. The yields of CO2 from FBP were much higher than those from MWAP at 450–850 °C. Whereas the yields of H2, CO and CH4 from MWAP were greater than those from FBP at higher temperature (e.g. 850 °C). The maximum condensate yields of FBP and MWAP were observed at 650 °C. Pyrolysis oil of MWAP contained less of macromolecules compared to FBP. Pyridine, phenol, aniline and their derivatives were major components in MWAP oil. Pyridine was the dominant oil component at 850 °C for FBP. Most of nitrogen-, sulfur- and chlorine-containing compounds were retained in FC (FBP char) and MC (MWAP char), and higher relative proportion (RP) of nitrogen, sulfur and chlorine were observed in the condensate and non-condensable gas from MWAP in comparison with FBP. FBP and MWAP both decreased risk degrees of heavy metals compared to raw DS, and heavy metals in FC and MC posed slight risk to the environment based on national standards in China.

The compound N-(4,6-dichloropyrimidine-2-yl)benzamide (C11H7Cl2N3O) was synthesized and the corresponding structure was confirmed by 1H NMR, 13C NMR, HRMS, IR, and single-crystal X-ray diffraction. The compound crystallized in a monoclinic system with space group P 21/c, where a = 14.9156(6), b = 16.6291(8), c = 14.4740(6) Å, β = 95.160(2)°, V = 3575.5(3) Å3, Z = 12, Dc = 1.494 g∙cm−3, F(000) = 1632, μ(MoKa) = 3.182 mm−1, final R = 0.0870, and wR = 0.2331 with I > 2σ(I). The crystal structure was found to be stabilized by intermolecular hydrogen bonding interactions N–H···O and C–H···Cl. Furthermore, the results from biological assays indicated that the compound showed a similar protective effect on metolachlor injury in rice seedlings compared to fenclorim at a concentration of 4.0 mg∙L−1. Moreover, the compound exhibited an improved antifungal activity compared to pyrimethanil against S. sclerotiorum and F. oxysporum. Potentially, these results lay the foundation for the development of novel herbicide safeners and fungicides.

ATP-binding cassette transporters A1 (ABCA1) and G1 (ABCG1), and macrophage scavenger receptor, cluster of differentiation (CD)36, function as key mediators of cholesterol efflux and influx from macrophages. In addition, they are associated with foam cell formation and the development of atherosclerosis (AS). The aim of the present study was to investigate the effects of extracellular signal-regulated kinases 1/2 (ERK1/2) inhibition on lipid balance in oxidized-low-density lipoprotein (Ox-LDL)-stimulated rat macrophages, and to examine the role of ERK1/2 inhibitors in AS. Rat peritoneal macrophages were treated with Ox-LDL alone or in combination with an ERK1/2 inhibitor, U0126, and untreated cells served as controls. Ox-LDL-induced lipid accumulation was detected by DiI fluorescence and oil red O staining. In addition, the mRNA and protein expression levels of ABCA1, ABCG1 and CD36 were determined using polymerase chain reaction and western blotting, respectively. Treatment with Ox-LDL significantly increased lipid accumulation and upregulated the mRNA and protein expression levels of ABCA1, ABCG1 and CD36 in macrophages. The addition of U0126 resulted in a marked reduction of lipid deposition, upregulation of ABCA1/G1 expression and suppression of CD36 expression in Ox-LDL-stimulated macrophages. The results of the present study indicated a novel association between ERK1/2 signaling and lipid metabolism, thus suggesting that inhibition of ERK1/2 may be considered a promising therapeutic strategy against AS.

In this Letter, an efficient synthetic route to prepare polysubstituted thiophene derivatives was achieved via the Et 3 N-mediated (Claisen) rearrangement reaction from α-oxo S -methyl- S -propargyl ketenes, which were obtained through alkylation of β-oxodithioesters with propargylic bromides, followed by regioselective intramolecular cyclization.

A monolithic fiber of molecularly imprinted polymer (MIP) was prepared by in situ polymerization within the capillary with an inner diameter of 530 µm. It was carried out in 8 min by microwave irradiation using malachite green (MG) as a template molecule, α-methacrylic acid (MAA) as a functional monomer, acetonitrile (ACN) as a porogenic solvent, ethylene dimethacrylate (EDMA) as a crosslinker, azodiiso-butyronitrile (AIBN) as a thermal initiator. The resulted MIP fibers were pushed out from the capillary, eluted and inserted in the capillary again, which successfully used for the solid phase microextraction (SPME) procedure. The factors affecting the extraction of MG, such as the molar ratio of template/monomer (MG/MAA), concentration of NaCl, extraction and desorption time, and extraction and desorption solvents were investigated in detail. The selectivity of the MIP fibers was compared using MG analogues crystal violet (CV) and non-analogue Sudan II. It was also employed for the pretreatment of trace MG in the fish feed followed by high-performance liquid chromatography (HPLC) detection. Under the optimal conditions, the linear range of MG was 10-600 μg/L, the detection limit (LOD) was 1.23 μg/L and the recovery of spiked fish feed sample was 88.7∼113.9%.

The rare N-unsubstituted glucosamine (GlcNH(3)(+)) residues in heparan sulfate (HS) have important biological and pathophysiological roles. Because of their low natural abundance, the use of chemically generated, structurally defined, N-unsubstituted heparin/HS oligosaccharides can greatly contribute to the investigation of their natural role in HS. However, the sequencing of mixtures of chemically generated oligosaccharides presents major challenges due to the difficulties in separating isomers and the available detection methods. In this study, we developed and validated a simple and sensitive method for the sequence analysis of N-unsubstituted heparin/HS oligosaccharides. This protocol involves pH 4 nitrous acid (HNO(2)) degradation, size-exclusion HPLC and ion-pair reversed-phase liquid chromatography-ion trap/time-of-flight mass spectrometry (IPRP-LC-ITTOF MS). We unexpectedly found that absorbance at 232 nm (normally used for specific detection of C4-C5 unsaturated oligosaccharides) was, in most cases, still sufficiently sensitive to also simultaneously detect saturated oligosaccharides during HPLC, thus simplifying the positional analysis of GlcNH(3)(+)) residues. The IPRP-LC-ITTOF MS system can supply further structural information leading to full sequence determination of the original oligosaccharide. This new methodology has been used to separate and sequence a variety of chemically generated, N-unsubstituted dp6 species containing between 1 and 3 GlcNH(3)(+)) residues per oligosaccharide in different positional combinations. This strategy offers possibilities for the sequencing of natural N-unsubstituted oligosaccharides from HS and should also be applicable, with minor modification, for sequencing at N-sulfated residues using alternative pH 1.5 HNO(2) scission.

Twenty-one phenylpropanoids, including 1 new (1) and 20 known phenylpropanoids (2–21), were isolated and identified from the fruits of Nicandra physaloides. The structures of these compounds were established by 1D and 2D NMR spectra referring to the literatures, together with mass spectrometry. It was found that the isolated compounds, except for 7, 18 and 19, showed the different levels of inhibitions on NO production by LPS-induced RAW 264.7 cells at IC50 values from 27.0 to 97.3 μM.

Background: Blocking angiogenesis by targeting vascular endothelial growth factor (VEGF) signaling pathway to inhibit tumor growth has proven to be successful in treating a variety of different metastatic tumor types, including kidney, colon, ovarian, and lung cancers, but its role in castration-resistant prostate cancer (CRPC) is still unknown. We here aimed to determine the efficacy and toxicities of anti-VEGF agents in patients with CRPC. Materials and Methods: The databases of PubMed, Web of Science and abstracts presented at the American Society of Clinical Oncology up to March 31, 2014 were searched for relevant articles. Pooled estimates of the objective response rate (ORR) and prostate-specific antigen (PSA) response rate (decline ≥50%) were calculated using the Comprehensive Meta-Analysis (version 2.2.064) software. Median weighted progressionfree survival (PFS) and overall survival (OS) time for anti-VEGF monotherapy and anti-VEGF-based doublets were compared by two-sided Student’s t test. Results: A total of 3,841 patients from 19 prospective studies (4 randomized controlled trials and 15 prospective nonrandomized cohort studies) were included for analysis. The pooled ORR was 12.4% with a higher response rate of 26.4% (95%CI, 13.6-44.9%) for anti-VEGF-based combinations vs. 6.7% (95%CI, 3.5-12.7%) for anti-VEGF alone (p=0.004). Similarly, the pooled PSA response rate was 32.4% with a higher PSA response rate of 52.8% (95%CI: 40.2-65.1%) for anti-VEGF-based combinations vs. 7.3% (95%CI, 3.6-14.2%) for anti-VEGF alone (p

A series of 3-phenyl benzo[d][1,2,3]triazin-4(3H)-one derivatives were synthesized through the condensation of phenol E and alkyl (alkenyl, alkynyl) chlorides (bromides, iodide) or alkyl chloroacetates or N-alkyl chloroacetamides using K2CO3 as the acid acceptor in N,N-dimethylformamide. Phenol E was prepared from starting material, 5-amino-2-chloro-4-fluorophenyl ethyl carbonate, in four steps involving in amidation, reduction, diazotization, and deprotecting-group reaction. The herbicidal activities of the title compounds were tested against two dicotyledonous plants and two monocotyledonous plants, in which some of them exhibited high herbicidal activities against two dicotyledonous plants in preemergence and postemergence treatments. Moreover, when the dosage was decreased to 180 and 90 g/ha, compounds F1, F8, and F9 showed highly selective inhibitory activities against amaranth pigweed, alfalfa, asteraceae, field sowthistle, morning glory, purslane, and velvetleaf in postemergence treatment but had no herbicidal efficacy on rape except F1, suggesting that it be possible to find a kind of herbicides to inhibit dicotyledonous weeds in the field of dicotyledonous crops with the same genus as aforementioned weeds.

A convenient base-mediated strategy to synthesize 3-aryol-4-methyl (or benzyl)-2-methylthio furans 2 (trisubstituted furans) has been developed through the domino coupling/annulations between available α-oxo ketene dithioacetals 1 and propargyl alcohols. In this strategy, these types of bases play an important role in driving the domino coupling reaction of propargyl alcohols and further intramolecular annulations to realize the target compounds. The possible mechanism for the formation of the various products is believed to involve the generation of allenes 7, followed by intramolecular annulations.

Microwave-assisted pyrolysis of furfural residue (FR) in an auger reactor was conducted. The biochar yield decreased and non-condensable gas yield increased with increasing temperature. Condensate yield reached maximum (i.e. 21.49 wt%) at 550 °C. Kaolin, CaO and K2CO3 enhanced tar secondary reactions, reduced the yield and O/C ratio of bio-oil, improved GC-MS areas of phenolic compounds to 76.25%, 89.28% and 93.1%, respectively. All additives improved yields of H2 and CH4, while CaO reduced CO2. With increasing temperature, relative proportion (RP) of HCN/NH3 reached up to 13.67, while RP of H2S and chlorine in volatiles increased from 1.17%, 5.97% to 2.75%, 9.00%, respectively. Ammonia nitrogen in volatiles increased to 6.94% by K2CO3. Kaolin improved RP of HCN from 0.11% to 5.47%, while K2CO3 eliminated HCN. H2S increased with kaolin addition and decreased with CaO and K2CO3. Electricity consumption of MWAP varied from 0.5 to 3.78 (kWh/kg FR) depending on temperatures and additives.

BACKGROUND Pyrazole oxime ether derivatives with different substituted pyridyl rings represent new types of compounds that possess good insecticidal and acarcidal activity against Aphis laburni Kaltenbach and Tetranychus cinnabarinus. RESULTS In total, 82 novel pyrazole oxime ether derivatives were synthesized and identified by 1H NMR, elemental analysis or high-resolution mass spectrometry, and their insecticidal and acarcidal activities were tested against A. laburni Kaltenbach and T. cinnabarinus. Bioassays showed that at a 200 mg L−1 dosage, one-third of the compounds displayed high insecticidal activity against A. laburni Kaltenbach (> 90%), whereas most of of the compound II series exhibited excellent acarcidal activity against T. cinnabarinus (> 92%). Most compound II series exhibited good activity in both insecticidal and acarcidal tests. In addition, at a low concentration of 10 mg L−1, the insecticidal activity of compounds IB9 and IE4 exceeded 90%, and the acarcidal activity of compounds IIB1 and IIB2 was ≥ 95%. CONCLUSION Structure–activity relationships were also examined. Results suggested that the tert-butoxycarbonyl group, as well as the position between tert-butoxycarbonyl and the atom N of the pyridyl ring, were essential to obtaining the acarcidal activity of the title compounds. © 2013 Society of Chemical Industry

A variety of novel 3-(α-hydroxymethylene)pyrrolidine-2,4-dione derivatives containing a cyclopropane moiety were designed and synthesized in satisfactory yields. Their structures were confirmed by 1H NMR and HRMS. The bioassays indicated that most of the title compounds displayed some extent herbicidal activities at 100 mg/mL.

A molecularly imprinted polymer (MIP) was prepared in acetonitrile by bulk polymerization, using di-n-octylphthalate (DOP) as a template molecular,α-methacrylic acid (MAA) as a functional monomer, and ethylene dimethacrylate (EDMA) as a crosslinker. Characterization and evaluation of the prepared MIP were carried out by scanning electron microscope (SEM), infrared absorption spectroscopy (IR), and the Scatchard analysis, respectively. Through the optimization of washing solvent, eluting solvent amount, flow rate of loading solution, and loading sample volume, an analysis method was established for DOP related compounds with high selectivity and sensitivity by using the selective molecularly imprinted solid-phase extraction (MI-SPE) technique. Moreover, under the optimal conditions, the extraction effects were comparatively investigated by using MIP cartridge, NIP cartridge, and the commercial PLS cartridge used especially for phthalic acid esters (PAEs), respectively. The results showed that the recoveries of spiked PAEs are in the range of 90.4%–97.8% with the relative standard deviation (RSD) of 1.6%–3.8% on the resulted MIP cartridge, whilst lower recoveries were obtained ranging from 80.2% to 88.9% with an RSD of 1.4%–5.2% on the commercial PLS cartridge.

A highly enantioselective palladium-catalyzed [3 + 2] cycloaddition of propargylic esters with β-ketoesters has been realized by employing a newly developed chiral ferrocene/benzimidazole-based P,N-ligand. This protocol features a good tolerance of functional groups in both propargylic esters and β-ketoesters, thereby delivering a variety of highly functionalized chiral 2,3-dihydrofurans bearing an exocyclic double bond at the 3-position in good yields and with high enantioselectivities (up to 98% ee).

In this Letter, an efficient synthetic route to prepare polysubstituted thiophene derivatives was achieved via the Et 3 N-mediated (Claisen) rearrangement reaction from α-oxo S -methyl- S -propargyl ketenes, which were obtained through alkylation of β-oxodithioesters with propargylic bromides, followed by regioselective intramolecular cyclization.

A series of novel N-(4-(2-aryloxythiazol-5-yl)but-3-yn-2-yl)benzamide derivatives were designed and synthesized. Their structures were identified by 1H NMR and elemental analyses. Preliminary bioassays indicated that some title compounds provided >80% control of Sclerotinia sclerotiorum at 50 µg/mL and >70% herbicidal activities against B. campestris at 100 µg/mL. Their structure-activities relationships were also discussed.

Melamine imprinted polymers (MIPs) have been prepared using identical polymer formulation by both thermal- and photo-initiation method, respectively. Physical characterization of the polymers revealed that the different polymerization methods led to the slight differences in both polymer structures and performance by scanning electron microscope (SEM), infrared absorption (IR), and mercury analyzer (MA). Both MIPs were used as selective sorbents for the solid phase extraction (SPE) of melamine in milk powders, followed by the determination coupled to HPLC. The recoveries of melamine in spiked milk powders were obtained in the range of 92.4-97.7% and 94.6-99.7%, for both MIPthermal and MIPphoto, respectively.

The commercially available ferrocene-based diphosphine ligand (Sc,SFc)-TaniaPhos was found to be highly effective in the Rh-catalyzed asymmetric hydrogenation of 3-aryl-2-(phosphonomethyl)propenates. Excellent enantioselectivity (90–98% ee) and high catalytic activity (S/C up to 1000) have been achieved, which represents the best results reported so far.

BACKGROUND: 4-(3-Trifluoromethylphenyl)pyridazine represents a new series of compounds with bleaching and herbicidal activities. RESULTS: A total of 43 novel 3-(substituted benzyloxy or phenoxy)-6-methyl-4-(3-trifluoromethylphenyl)pyridazine derivatives were synthesised, and their bleaching and herbicidal activities were evaluated through Spirodela polyrrhiza and greenhouse tests. Some compounds exhibited excellent herbicidal activities, even at a dose of 7.5 g ha−1. CONCLUSION: The results showed that a substituted phenoxy group at the 3-position of the pyridazine ring and the electron-withdrawing group at the para-position on the benzene ring were essential for high herbicidal activity. Copyright © 2011 Society of Chemical Industry