Synthesis,Characterization, and Catalytic Behavior of Bamboo Rice Husk Ash

In this paper, we report the use of bamboo rice husk ash as an efficient, greener, reusable, and biodegradable heterogeneous catalyst for the synthesis of tetrahydro‐4H ‐chromene‐3‐carbonitriles via the one‐pot three‐component reaction of malononitrile with aromatic aldehydes and dimedone or 1,3‐cyclohexanedione. The formation of bamboo rice husk ash‐silica has been confirmed by several analytical techniques.     

Nano Silicon from Nano Silica Using Natural Resource (Rha) for Solar Cell Fabrication

Abstract

High purity (～99%) nano silica with an average particle size of ～100 nm was extracted at pH 3 at 650°C from a natural resource, rice husk, using alkaline extraction followed by acid precipitation method. Using nano silica as a precursor, silicon (Si) nanoparticles have been synthesized by high-temperature magnesiothermic reduction method. The prepared sample was characterized by X-ray diffraction, particle size analyzer, Fourier transform infrared spectroscopy, transmission electron microscopy, X-ray fluorescence analyzer, and UV–Vis spectroscopy. The comprehensive characterization studies indicate the pure phase formation of Si and the variation of particle size from 70 nm to 100 nm for samples synthesized at different sintering temperatures. Moreover, the silicon nanoparticles produced at 850°C have pure phase formation, high purity, and good absorption peaks. The efficiency calculated through IV characteristics is found to be increasing in silicon and ruthenium combination (2.67%), which is better than that achieved from the conventional solar cells. The produced silicon nanoparticles could be applied as an anode material for solar cell fabrication.     

Synthesis and Biological Evaluation of the Forssman Antigen Pentasaccharide and Derivatives by a One‐Pot Glycosylation Procedure

The synthesis and biological evaluation of the Forssman antigen pentasaccharide and derivatives thereof by using a one‐pot glycosylation and polymer‐assisted deprotection is described. The Forssman antigen pentasaccharide, composed of GalNAcα(1,3)GalNAcβ(1,3)Galα(1,4)Galβ(1,4)Glc, was recently identified as a ligand of the lectin SLL‐2 isolated from an octocoral Sinularia lochmodes. The chemo‐ and α‐selective glycosylation of a thiogalactoside with a hemiacetal donor by using a mixture of Tf₂O, TTBP and Ph₂SO, followed by activation of the remaining thioglycoside, provided the trisaccharide at the reducing end in a one‐pot procedure. The pentasaccharide was prepared by the α‐selective glycosylation of the N‐Troc‐protected (Troc=2,2,2‐trichloroethoxycarbonyl) thioglycoside with a 2‐azide‐1‐hydroxyl glycosyl donor, followed by glycosidation of the resulting disaccharide at the C3 hydroxyl group of the trisaccharide acceptor in a one‐pot process. We next applied the one‐pot glycosylation method to the synthesis of pentasaccharides in which the galactosamine units were partially and fully replaced by galactose units. Among the three possible pentasaccharides, Galα(1,3)GalNAc and Galα(1,3)Gal derivatives were successfully prepared by the established method. An assay of the binding of the synthetic oligosaccharides to a fluorescent‐labeled SLL‐2 revealed that the NHAc substituents and the length of the oligosaccharide chain were both important for the binding of the oligosaccharide to SLL‐2. The inhibition effect of the oligosaccharide relative to the morphological changes of Symbiodinium by SLL‐2, was comparable to their binding affinity to SLL‐2. In addition, we fortuitously found that the synthetic Forssman antigen pentasaccharide directly promotes a morphological change in Symbiodinium. These results strongly indicate that the Forssman antigen also functions as a chemical mediator of Symbiodinium.     

神府煤与稻杆共热溶研究

研究了神府煤与稻杆在1-甲基萘溶剂中不同温度下的共热溶行为。相对神府煤,稻杆单独热溶时具有更高的热溶率,表明其具有较好的热溶活性。但稻杆的热溶过程中产生大量的挥发性气体,导致其热溶率和热溶物产率之间的较大差异。神府煤单独热溶时,其热溶率与热溶物产率之间的差异相对较小。神府煤与稻杆的共热溶表明,两者之间存在协同效应,并且该协同效应受温度的影响显著。在热溶温度为320~340 ℃时,对热溶物产率而言具有正的协同效应,也即其热溶物产率的实验值大于通过神府煤与稻杆单独热溶时热溶物产率经质量加权平均计算得到的理论值。在研究的热溶温度范围内,共热溶的热溶率实验值均低于质量加权平均的理论计算值。相对于理论计算值,在320 ℃时热溶物产率的实验值增加达到最大,为7.9%。此外,通过对热溶物的性质表征,还进一步探讨了共热溶过程中的协同作用机理。     

混合型固相萃取-高效液相色谱-串联质谱法测定稻米中3种谷维素北大核心CSCD

建立了利用高效液相色谱-串联质谱结合混合型阴离子交换固相萃取柱测定稻米中3种谷维素(环木菠萝烯醇阿魏酸酯(CA-FA)、24-亚甲基环木菠萝烯醇阿魏酸酯(24MCA-FA)和菜油甾醇阿魏酸酯(Camp-FA))含量的分析方法。实验通过优化3种谷维素的多反应监测(MRM)质谱参数,比较了在不同流动相中的分离度以及响应强度,同时考察了不同提取条件、净化条件对3种谷维素提取率和净化效果的影响,再结合外标法定量,实现了对稻米中3种谷维素的定量分析。实验结果表明,采用5 mmol/L乙酸铵水溶液为流动相A,甲醇∶乙腈=1∶1(v/v)为流动相B,梯度洗脱,3种谷维素在Agilent Eclipse XDB-C8色谱柱(150 mm×2.1 mm,3.5μm)上基本分离且响应强度和峰形最佳;提取条件经正交实验优化后可得:料液比为1∶20(g/mL)、提取溶剂为甲醇、浸泡时间为12 h、超声温度为40℃以及超声时间为20 min时,3种谷维素提取率最高;对混合型阴离子交换固相萃取柱的上样溶剂以及洗脱溶剂优化后,样品基质效应为1.6%~10.8%。在各优化条件下,3种谷维素在各自的线性范围内线性良好,相关系数(r2)均≥0.9983,检出限(LOD)为0.5~1.0μg/L,定量限(LOQ)为2.0~3.5μg/L。在稻米样品本底浓度2、5和10倍的加标水平下3种谷维素的平均回收率为86.1%~110.6%,相对标准偏差(RSD)为0.9%~3.2%。该方法可快速准确测定稻米中3种谷维素的含量,为后续稻米中谷维素类化合物测定及鉴定奠定基础。     

Optimizing pyrolysis temperature of contaminated rice straw biochar: Heavy metal(loid) deportment,properties evolution,and Pb adsorption/immobilization

Pyrolysis of rice straw (RS), a popular method for producing biochar, effectively treats heavy metal(loid)-contaminated RS. Here, we carried out this process at different temperatures and investigated the deportment of heavy metal(loid)s and the property evolution of biochars. Also, the optimal pyrolysis temperature for Pb adsorption and immobilization was studied. We observed that increasing the temperature could volatilize the heavy metal(loid)s. Cd was the most volatile metal therein, followed by As, while Ni, Cu, and Pb were relatively refractory. More than 75% of the remaining heavy metal(loid)s were non-exchangeable fractions at 700 °C, significantly reducing the environmental risk during subsequent application. Meanwhile, higher pyrolysis temperature resulted in higher pH values, higher surface areas, and stronger Pb adsorption capacity of RS biochars. The maximum adsorption capacity (Q_m) of biochars was in the order of BC300 (77.2 mg·g^?1) < BC500 (137.2 mg·g^?1) < BC700 (222.6 mg·g^?1). Besides, high-temperature biochar could significantly reduce the vertical Pb migration. And BC700 increased the fraction of residual Pb from 39.7% to 44.0% in the soil under the acid rain leaching condition. Therefore, we propose that the heavy metal(loid)-contaminated RS biochar produced at 700 °C might be more suitable for the remediation of soil heavily polluted in the Pb-smelting area.     

超高效液相色谱-串联质谱快速检测精米、玉米与土豆样品中噻呋酰胺残留

采用分散固相萃取(QuEChERS)为样品前处理方法,建立了超高效液相色谱-串联质谱(UPLCMS/MS)快速检测精米、玉米和土豆中噻呋酰胺残留的分析方法。样品经乙腈提取,PSA净化,超高效液相色谱分离,电喷雾电离、负离子扫描,三重四极杆串联质谱以多反应监测扫描方式进行检测,基质匹配标准品外标法进行定量分析。结果显示,噻呋酰胺在1.0~1 000μg·L-1范围内呈良好线性(r2=0.999 0)。在0.01~1.0 mg·kg-1加标水平范围内,噻呋酰胺在精米、玉米和土豆中的平均回收率为89.1%~109.3%,相对标准偏差为3.5%~8.7%,检出限(LOD)为0.009~0.015μg·kg-1,定量下限(LOQ)为0.032~0.049μg·kg-1。该方法简便、快速、准确,可用于精米、玉米和土豆中噻呋酰胺农药残留的确证检测。     

HPLC法同时测定黄酒中4种非法食品添加剂

建立高效液相色谱同时测定黄酒中安赛蜜、苯甲酸、山梨酸和糖精钠4种非法食品添加剂的方法。黄酒中的待测物质经提取后,采用C18柱分离,以甲醇–乙酸铵溶液为流动相进行洗脱,在波长230 nm处用高效液相色谱–二极管阵列检测器进行测定。安赛蜜、苯甲酸、山梨酸和糖精钠的质量浓度在0.5～200.0μg/mL范围内与其色谱峰面积的线性关系良好(r0.999 7),检出限为0.29～0.74μg/L。在0.5,1.0,2.5,5.0,7.5 mg添加水平时的平均回收率在95.6%～104.0%范围内,测定结果的相对标准偏差为0.3%～1.5%(n=6)。该方法操作简便,分离效果好,灵敏度高,结果稳定可靠,适合于黄酒中安赛蜜、苯甲酸、山梨酸和糖精钠的同时测定。     

磺酰脲类化合物在水稻田中的除草性能

水稻是我国重要的粮食作物,但杂草对水稻的产量和品质产生了严重影响。 化学防除是治理水稻田杂草最有效的途径。 文中设计合成了苯环2,6-取代和2,5-取代两个系列磺酰脲类化合物,并通过核磁共振波谱仪(NMR)和高分辨质谱仪(HRMS)等对其进行了结构表征。 通过水稻田除草活性和安全性测试发现化合物在水稻田中具有较好的除草活性,尤其是化合物10a对水稻田中的主要杂草稗草和醴肠除草活性(目测初筛防效大于90%)优于对照药醚苯磺隆和氯磺隆,安全性与之相当。