Synthesis, Crystal Structure and Fungicidal Activity of 3-(Difluoromethyl)-1-methyl-N-((2-(trifluoromethyl)phenyl) carbamoyl)-1H-pyrazole-4-carboxamide

The title compound 3-(difluoromethyl)-1-methyl-N-((2-(trifluoromethyl)phenyl)-carbamoyl)-1 H-pyrazole-4-carboxamide(C14 H11 F5 N4 O2) was synthesized, and its structure was confirmed by 1 H NMR, H RMS and X-ray diffraction. It crystallizes in monoclinic system, space group P21/n with a = 6.994(3), b = 13.860(6), c = 15.308(7)A,β= 97.632(6)°, V = 1470.8(11) A^3,Z = 4, the final R = 0.0692 and wR = 0.2108 for 3989 observed reflections with Ⅰ> 2σ(Ⅰ). The preliminary biological test shows that the title compound has moderate fungicidal activities against Pseudomonas syringae.

Determination of sulfur anions by ion chromatography-postcolumn derivation and UV detection

A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All species are separated at Dionex IonPac AG22A and AS22A with mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0 mL/min. The postcolunm derivation solution was 0.24% iodine in 0.2% phosphate acid and the detection wavelength was set at 288 nm. The detection limits （LOD, signal-to-noise ratio of 3） of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate were 0.004, 0.006, 0.006, and 0.007 mg/L, respectively. Within-day relative standard deviations （RSD, n = 10） of formaldehyde sulfoxylate, sulflte, thiocyanate, and thiosulfate were 3.24%, 3.76%, 2.68%, and 2.07%, respectively. The recoveries of the four anions were in the range of 67.2-116.5%.

Purification and characterization of keratinase from a new Bacillus subtilis strain

The aim of this study was to purify and characterize a keratinase produced by a new isolated Bacillus subtilis KD-N2 strain. The keratinase produced by the isolate was purified using ammonium sulphate precipitation, Sephadex G-75 and DEAE (diethylaminoethyl)-Sepharose chromatographic techniques. The purified enzyme was shown to have a molecular mass of 30.5 kDa, as determined by sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) analysis. The optimum pH at 50 °C was 8.5 and the optimum temperature at pH 8.5 was 55 °C. The keratinase was partially inactivated by some metal ions, organic solvents and serine protease inhibitor phenylmethanesulfonyl fluoride (PMSF). Sodium dodecyl sulfate (SDS) and ethylene diamine tetraacetic acid (EDTA) had positive effect on the keratinase activity. Reducing agents including dithiothreitol (DTT), mercaptoethanol, L-cysteine, sodium sulphite, as well as chemicals of SDS, ammonium sulfamate and dimethylsulfoxide (DMSO) stimulated the enzyme activity upon a feather meal substrate. Besides feather keratin, the enzyme is active upon the soluble proteins ovalbumin, bovine serum albumin (BSA), casein and insoluble ones as sheep wool and human hair. Calf hair, silk and collagen could not be hydrolyzed by the keratinase.

Synthesis, Crystal Structure and Biological Activity of a New 1,2,4-Triazole Derivative

A new 1,2,4-triazole containing cyclopropane moiety was synthesized and characterized by 1H NMR, MS and elemental analyses. The crystal structure of the title compound （C13H14FN3S, Mr= 263.33） has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.614（3）, b = 7.0202（14）, c = 15.556（3）A, β = 110.92（3）°, V = 1286.7（4） A3, Z = 4, F（000） = 552, D,. = 1.359 g/cm3,μ = 0.25 mm-1, the final R = 0.0336 and wR = 0.0898 for 2568 observed reflections with 1 〉 2σ（/）. A total of 10093 reflections were collected, of which 3045 were independent （Rint = 0.0268）. The herbicidal activity of the title compound was determined, and this compound displays excellent herbicidal activity against Brassica campestris.

Synthesis,Crystal Structure and Antifungal Activity of N-((2,6-Difluorophenyl)carbamoyl)-1,3-dimethyl-1H-pyrazole-4-carboxamide

The title compound N-（（2,6-difluorophenyl）carbamoyl）-1,3-dimethyl-1 H-pyrazole-4-carboxamide（C13H12F2N4O2） was synthesized, and its structure was confirmed by ^1H NMR,HRMS and X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 9.50（2）, b = 10.11（2）, c = 14.07（3） A^°, β = 102.15（3）°, Dc = 1.480 g/cm^3, Z = 4, V = 1320（5） A^°3, the final R = 0.0789 and wR = 0.1860 for 1054 observed reflections with I 〉 2σ（I）. The preliminary biological test shows that the title compound has weak antifungal activities.

Microwave Assistant Synthesis,Crystal Structure and Biological Activity of 1-(2-Fluorobenzyl)-3-methoxy-4-methyl-1H-1,2,4-triazol-5(4H)-one

The title compound 1-（2-fluorobenzyl）-3-methoxy-4-methyl-lH-1,2,4-triazol- 5（4H）-one （CI1HI2FN302） was synthesized, and its structure was confirmed by 1H NMR, IR, MS, elemental analysis and X-ray diffraction. It crystallizes in the monoclinic system, space group Pi with a = 6.919（3）, b = 8.525（4）, c = 9.811（4） A, a = 84.22（2）, β = 71.028（19）, γ = 86.10（2）°, Dc = 1.448 g/cm3, Z = 2, V= 544.2（4） A3, F（000） = 248, the final R = 0.0379 and WR = 0.0913 for 1709 observed reflections with I〉 2σ（I）. The preliminary biological test shows that the title compound shows weak inhibitory activities against Phytophthora infestans, Botrytis cinerea, Corynespora cassiicola, Rhizoctonia solani and Pythium ultimum.

Hydrolysis Lignin as a Sorbent and Basis for Solid Composite Biofuel

New powdered sorbent Lignosorb based on the hydrophobized hydrolysis lignin has been developed at the Belarusian State University. Hydrolysis lignin is a commercial waste product of biomass processing in the hydrolysis production of ethanol. In spite of the various proposals for hydrolysis lignin usage, the wide application has not found yet. Special area of hydrophobized hydrolysis lignin usage as a sorbent for oil spills removal and oil products waste recovery is discussed. Lignosorb, thanks to the rather high bulk density, can be applied manually or mechanically by conventional sprayers. It does not sink after oil adsorption and transforms liquid oil film on the water surface into the solid mass. The solid product is a complete mass and is easily collected from the surface of water. Lignosorb when blended with oil products waste in the volume forms the granular free-running product. The rheological properties of the Lignosorb suspensions in oil products at different sorbent to oil product ratio have been estimated. Saturated by different oil products Lignosorb one can granulate or pellet and utilize as a composite solid fuel including the co-firing regime of combustion. It has the higher heating value of 32.1 - 38.8 MJ/kg while the coal has 20.9 - 30.1 MJ/kg. It has been shown that composite fuel burning has less longstanding inflammation stage, more long stable burning stage and less longstanding phase of smoldering in the comparison to wood and Lignosorb burning.

Antihypertensive Properties on Spontaneously Hypertensive Rats of Peptide Hydrolysates from Silkworm Pupae Protein

Peptide hydrolysates of silkworm pupae protein with molecular weight of less than 5000 Da were prepared by ultrafiltration. The extracted peptide hydrolysates of silkworm pupae protein had inhibitory action on angiotensin-I-converting enzyme activity in vitro. The hydrolysates were orally administered to spontaneously hypertensive rats (SHR) in one period and long-term (four weeks). The results showed that the systolic blood pressure (SBP) of the treatment groups decreased in a dose-related manner. After one oral administration of silkworm protein hydrolysates with doses of 60, 20 and 5 mg/kg, the SBP of SHR decreased by 21.5, 13.8, and 9.0 mmHg in 1.5 h. After four weeks of the treatment in 80 mg/kg, the SBP decreased by 25 mmHg, with the antihypertensive activity close to 4 mg/kg of captopril;the SBP of the 40 mg/kg dose group also decreased by 17.5 mmHg. The peptide hydrolysate did not affect the SBP in normal, non-hypertensive rats in one period and long-term treatments. The acute toxicity research showed that the peptide hydrolysates were safe and without side effects. This research would be helpful in exploring the silkworm protein peptides as functional components for the antihypertension treatment.

Total synthesis of glypetelotine

glypetelotine 的全部的合成，从 Glycosmis petelotii 的叶摘录的第一包含硫的吲哚碱在越南的北方收集了，通过 6 步从吲哚被描述。glypetelotine 的结构被红外证实， 1 H NMR， 13 C NMR 和 MS 分析。光谱合成化合物的数据与自然化合物的那些是相同的。

Hazardous and Harmful Factors on Construction Sites and Their Prevention

In this paper, the status quo of safety production on construction sites and the hazardous and harmful factors in the construction process were analyzed, and corresponding suggestions were proposed to make up for the shortcomings of the safety production assurance system standards on construction sites.

Rheological Properties of Casting Solutions for Starch Edible Films Production

Rheological properties of corn starch and sodium alginate blend solutions have been measured at different polymer ratios in the temperature range from 303 to 343 K bya R/S Brook field rheometer with аcoaxial cylinder measuring unit. Dynamic viscosity of blends has been shown to decrease with shear rate increase and to increase with sodium alginate content increase. The influence of shear rate on activation energy of viscous flow depends on sodium alginate content and is different for below and over 5% (mass) content. Applicability of Ostwald-de-Waele, Herschel-Bulkley, Bingham and Casson models for the description of CS:SA blend solutions flow has been analyzed. Rheological properties of CS:SA blend solutions allow one to look at them as an alternative to starch solutions for edible films casting and production by dry method.

MicroR-9c-5p and novel-mir50 co-target Akt to regulate Lasioderma serricorne reproduction

High fecundity is a common characteristic of insect pests which increases the difficulty of population control.Serine/threonine kinase Akt is an indispensable component of the insulin signaling pathway.Silencing of LsAkt severely hinders reproduction in Lasioderma serricorne,a stored product insect pest.However,the post-transcriptional pathway of LsAkt in L.serricorne remains unknown.This study identified 2 binding sites of miR-9c-5p and novel-mir50 in the coding sequences of LsAkt.The expression profiles of 2 microRNAs(miRNAs)and LsAkt displayed an opposite pattern during the adult stages.Luciferase reporter assay showed that novel-mir50 and miR-9c-5p could downregulate the expression of LsAkt.Overexpression of miR-9c-5p and novel-mir50 by injection of mimics inhibited the expression of LsAkt and reduced oviposition,decreased egg hatchability,and blocked ovarian development.It also decreased the expression of genes involved in ovarian development(LsVg and LsVgR)and the nutritional signaling pathway(LsTOR,LsS6K,and Ls4EBP),and reduced the phosphorylation of Akt.Conversely,injection of miR-9c-5p and novel-mir50 inhibitors induced the expressions of LsAkt,LsVg,LsVgR,LsTOR,LsS6K,and Ls4EBP,enhanced Akt phosphorylation level,and accelerated ovarian development.Injection of bovine insulin downregulated the expression of miR-9c-5p and novel-mir50 and upregulated the LsAkt expression.It also rescued the reproductive development defects associated with miR-9c-5p/novel-mir50 overexpression,forming a positive regulatory loop of insulin signaling.These results indicate that miR-9c-5p/novel-mir50 regulates the female reproduction of L.serricorne by targeting Akt in response to insulin signaling.The data also demonstrate the effects of the insulin/miRNA/Akt regulatory axis in insect reproduction.

Visible-light-enabled multicomponent synthesis of trifluoromethylated 3-indolequinoxalin-2(1H)-ones without external photocatalysis

A novel and sustainable visible-light-enabled multicomponent reaction involving quinoxalin-2(1H)-ones,indoles,and CF3SO2Na that does not require an external photocatalyst is described.This photoinduced reaction employs air as the sole oxidant,thereby providing a green and highly step-efficient approach to a series of biologically important trifluoromethylated 3-indolequinoxalin-2(1H)-ones.

Anti-corrosive mechanism of poly(N-ethylaniline)/sodium silicate electrochemical composites for copper:Correlated experimental and in-silico studies

Poly(N-ethylaniline)(PNEA)composites with varying silicate content were fabricated on copper through a novel electropolymerized strategy in acidic solution.Thickness,compactness,conductivity and adhesive strength of the composite(PNEA-10 Si)were optimized as silicate content reached 10 m M.Electrochemical,morphological and solution analyses were employed to evaluate the protective performance of PNEA and PNEA-10 Si coatings for copper in 3.5%Na Cl solution.Results of electrochemical analyses indicated that as-prepared coatings retarded the oxygen reduction process efficiently for copper in 3.5%Na Cl solution,drained corrosion current density and elevated interfacial charge transfer resistance.Due to favorable barrier effect,compact structure and low porosity index,PNEA-10 Si composite exhibited superior anti-corrosive performance,which was more tolerant than PNEA during long-time immersion.PNEA-10 Si coated sample exhibited a stable topography after 144 h immersion with the minimum concentration of released ions revealing the improved protection capacity.Electronic/atomic-multiscale calculations were conducted to clarify the deposition and protection mechanism of as-prepared coatings.Outcomes of density functional theory corroborated that silicate is stabilized in the PNEA layer via electrostatic force;and immobile silicate positively contributed to the charge transfer barrier of the composite.Molecular dynamics simulations evidenced that the favorable compatibility between PNEA and silicate facilitated polymer deposition and confined in-situ ions diffusion.

Optimization strategies for Cd and Pb immobilization in soil using meta-analysis combined with numerical modeling

Chemical immobilization is one of the most effective technologies for remediating sites with heavy metals,but the selection of proper immobilization material and determination of its dose ratio is a challenge that limits the remediation efficiency.In this study,we conducted a meta-analysis of 489 independent observations on the immobilization of heavy metals,in which the immobilization materials were divided into biochar,phosphate,lime,metal oxides,and clay minerals.The statistical analysis of these observations revealed that the material dose ratio was the most important parameter that controlled immobilization efficiency,and the Freundlich adsorption model was successfully applied to calculate the bioavailable heavy metal(BHM)concentration after immobilization.Based on the calculation results,phosphate was the most effective material for Pb immobilization.Lime was the most effective when the initial bioavailable Cd content was 0.1–1 mg kg^(-1),whereas the immobilization effects of lime and phosphate were similar when the initial bioavailable Cd content was 10 mg kg^(-1).In addition to the material dose ratio,initial soil pH(pHi)and organic matter(OM)content were negatively correlated,whereas the fraction of initial BHMs before immobilization(FB)and immobilization time were positively correlated with immobilization efficiency.A numerical model that considered the material dose ratio,pHi,OM,FB,and immobilization time was established to calculate the residual BHM concentration after immobilization.However,these factors only explained less than 45%of the immobilization effect,indicating that other factors,such as the sub-type of the material and modification methods,also affect the immobilization effect.These results could help to optimize the type of immobilization material of heavy metals and its dose ratio in practical engineering applications.

Visible-light-induced C–H sulfenylation of quinoxalin-2(1H)-ones with disulfides by sustainable cerium catalysis

Using visible light as energy to form free radicals has important synthetic value.A novel and efficient visible-lightmediated strategy has been developed for the generation of thiobenzene radicals through cerium-catalyzed activation of the disulfides.Through this photochemical reaction,various 3-sulfenylated quinoxalin-2(1H)-ones can be conveniently obtained in good yields with good functional group tolerance.Our transformation provides an alternative that allows rapid access to various C3 sulfenylated quinoxalin-2(1H)-ones in a sustainable and practical manner.

Flavor profile variations of Huangjiu brewed in different traditional Chinese solar terms

Background:Through long-term research on Huangjiu fermentation,it has been found that the quality of Huangjiu is closely associated with Chinese 24-solar term.Therefore,this study was conducted to explore the characteristic and property index differences of Huangjiu,such as aroma and flavor profile,and physicochemical properties—brewed in different solar terms by choosing five representative fermentation times of Shaoxing Huangjiu.Results:Huangjiu samples in the current study all met the national standards of traditional semi-dry Huangjiu.There are significant differences in physicochemical properties such as acidity and amino nitrogen among different solar-term groups.Forty three detected volatiles were applied by principal component analysis and partial least squares discriminant analysis analyses to differentiate the main factors.Volatiles mainly loaded to four principal components,which accounted for 86.5%.Nineteen volatiles were discriminated to significantly differentiate solar-term groups.Odor activity values(OAV)analysis found 14 compounds with OAV>1,while correlation analysis between volatiles and the outcomes of sensory evaluation displayed the various properties of Huangjiu on aroma and flavor due to the various combinations of volatiles,reducing sugar,acidity and amino nitrogen.After a national wine inspector evaluated and scored Huangjiu fermented in different solar terms,Huangjiu brewed in Winter Solstice exhibited the highest performance,with a score of 91.0,and praised as a kind of gold medal product.Conclusion:The methodology of this study can help to produce more types of appealing flavor and aroma of alcoholic beverages to consumers,build varietal Huangjiu or other alcoholic beverages through fermenting guidance by solar term,and even expand the applications of the traditional Chinese 24-solar term.