超高效液相色谱法同时测定洋常春藤中8种成分含量

建立了同时测定洋常春藤中绿原酸、隐绿原酸、芦丁、烟花苷、常春藤皂苷C、常春藤皂苷D、常春藤皂苷B和α-常春藤皂苷8种成分的超高效液相色谱法(UHPLC)。以80%甲醇为溶剂,将药材粉末于85℃、料液比1∶100条件下水浴回流1 h,制备供试品溶液;采用Agilent ZORBAX Eclipse Plus-C_(18)(2.1 mm×100 mm,1.8μm)色谱柱,以乙腈-0.05%磷酸溶液为流动相进行梯度洗脱。结果表明,上述8种成分均获得良好的分离度;仪器精密度、方法重复性的相对标准偏差(RSD)均小于3.0%;样品溶液在室温条件下24 h内稳定;8种成分在对应质量浓度范围内线性关系良好(r≥0.999 5),检出限为0.40～10.58μg·mL~(-1),定量下限为1.31～34.61μg·mL~(-1),平均回收率为97.3%～108%,RSD(n=6)为0.51%～3.2%。该方法适用于洋常春藤中上述8种化学成分的定量分析。     

超亲水超疏油油水分离膜的制备及其性能

超亲水-超疏油油水分离膜是一种过水隔油的特殊分离膜,在处理海洋溢油污染、环境含油废水时具有保持分离膜不被油污染的优势,有十分重要的实际意义。为了掌握近年来超亲水超疏油分离膜的发展动态,本文首先以液体静压力与毛细作用力为基础阐述亲水疏油膜的油水分离机理;然后分类概括超亲水-超疏油金属基底网膜、刺激响应油水分离膜、无基底聚合物膜材料的制备及各项性能的研究新进展;最后总结目前在该领域仍存在的问题并进行展望。     

电感耦合等离子体质谱（ICP-MS）法测定食用植物油中铅和砷的含量

采用改进的微波消解-电感耦合等离子体质谱(ICP-MS)法,实现了对植物油中铅、砷的定量测定,弥补了微波消解植物油前处理不彻底的不足。铅、砷浓度在0～50μg/L范围内具有良好的线性关系(r≥0.999),相对标准偏差(RSD)为1.2%～4.9%,加标回收率为81.0%～109%,检出限分别为1.11μg/kg和0.90μg/kg,能满足现有标准的检测要求。     

火焰原子吸收法测定云母钛珠光颜料中6种重金属元素

本文采用硝酸/氢氟酸/盐酸混合酸消解,火焰原子吸收法测定云母钛珠光颜料中的Pb、Cd、Co、Cr、Cu、Ni 6种重金属元素的含量。各元素校正曲线的线性关系良好,相关系数在0.9991~0.9996之间,检出限在0.0018~0.0510 mg/L之间。平行测定7次,各元素的RSD均不大于1.21%。各元素在添加水平为0.5μg/mL时的回收率为88.9~107.6%之间。该方法获得了令人满意的测量效果,对云母钛珠光颜料中重金属含量的测定提供了可靠的分析方法。     

Structural-borne acoustics analysis and multi-objective optimization by using panel acoustic participation and response surface methodology

This paper is aimed to investigate the structural-borne acoustics analysis and multi-objective optimization of an enclosed box structure by using the panel acoustic participation (PAP) and response surface methodology (RSM). The acoustic frequency response function is applied to achieve the critical frequency of interest under each excitation. The PAP analysis is then carried out at all critical frequencies and the remarkable acoustic panels are identified. The correlation coefficient matrix method is proposed for reselecting and grouping the positions of acoustic panels identified to paste damping layer to control noise. With the help of faced central composite design, an efficient set of sample points are generated and then the second-order polynomial functions of sound pressure response at each critical frequency are computed and verified by the adjusted coefficient of multiple determination. The functional relationships between sound pressure responses and the thicknesses of damping layers are investigated, and multi-objective optimization of the thicknesses of damping layers is developed. The results indicate that, by using the PAP and RSM, the structural-borne acoustics at critical frequencies are calculated conveniently and controlled effectively. The optimization process of the explicit optimization model proposed in this paper is simple and the computational time is saved.     

Ultrasonic synthesis of two nanostructured cadmium(II) coordination supramolecular polymers: Solvent influence,luminescence and photocatalytic properties

Two nanoparticles of cadmium(II) coordination polymers (CPs) formulated as [Cd(L)(DCTP)]_n (1) and [Cd(L)₂(DCTP)·2H₂O]_n (2) (L = 1,2-bis(2-methylbenzimidazol-1-ylmethyl)benzene, H₂DCTP = 2,5-dichloroterephthalic acid) were prepared by the sonochemical approach in different solvents and characterized by elemental analysis, IR spectra, scanning electron microscopy (SEM), and powder X-ray diffraction. Structural determination reveals that CP 1 displays a 2D four-connected sql net layer, Whilst CP 2 exhibits a 1D “V”-like chain structure. Luminescence properties, thermal behavior, and photocatalytic activities of the nanoparticles of CPs 1 and 2 on the degradation of methylene blue were investigated. The photocatalytic mechanism is carried out by introducing t-butyl alcohol (TBA) as a widely used OH scavenger. Furthermore, the influence of solvents, reaction time, and ultrasound irradiation temperature on the morphology and size of the nanostructure CPs 1 and 2 were investigated. The results indicated that an increase of time and ultrasound irradiation temperature decreased the nanostructured size.     

残余应力的超声横纵波检测方法

基于声弹性原理,研究板材厚度方向、螺栓轴向方向(以下简称z轴方向)宏观残余应力分布的超声无损检测方法。针对被测构件厚度不均匀对应力检测精度的影响非常大、检测原理繁杂不适合工程应用、拉伸实验中拉伸形变对应力系数测量精度的影响很大等问题,采取超声横波、纵波相结合的方法重新推导检测公式,并提出采用一发一收模式进行拉伸实验,通过对实验数据进行拟合,由公式计算出声弹性系数代替应力系数。然后结合插值、互相关等算法,采用VC++编制z轴方向残余应力超声检测软件并搭建检测系统。分别对性能为A2-70,4.8,8.8,长度依次为135 mm,100 mm,100mm的M20的螺栓进行拉伸实验,比对计算拉伸应力与检测拉伸应力,结果表明,该测量系统的绝对误差限为20 MPa,相对误差小于25%,且应力值较大时,相对误差有所减小,当应力值大于100 MPa时,相对误差小于5%,非常实用。      

Application of the FEM/DEM and alternately moving road method to the simulation of tire-sand interactions

The three-dimensional finite-discrete element method (FEM/DEM) is applied to the simulation of tire-sand interactions, where the tire is discretized into hexahedron finite elements and sand is modeled by using the discrete element method. The feasibility and effectiveness of the method are proven by comparing the simulation results with the current reported results. Since long test roads are usually required for investigating tire running behaviors, which lead to large-scale simulation models and time consuming problems, the alternately moving road method is proposed to handle this problem. It can simulate tire running behaviors on an arbitrary length sand road with a constant road length value. The numerical model of a lug tire running on a bisectional road with fine and coarse sand is established to verify the feasibility of the method.     

Synthesis,insecticidal activities and structure–activity relationship study of dual chiral sulfilimines

To investigate the “methyl” impact on bioactivity of sulfiliminyl dicarboxamides, a total of 16 novel N-cyano and N-trifluoroacetyl sulfiliminyl dicarboxamides containing m-heptafluoroisopropylated aromatic amino moiety were studied. Two series of sulfiliminyl substituents were designed, synthesized and evaluated against oriental armyworm (Pseudaletia separata Walker) for their insecticidal activities. Their chemical structures were established by corresponding \(^{1}\hbox {H}\) NMR, HRMS and optical polarimetry. Bioassay results revealed that some of the title compounds showed potent insecticidal activities against oriental armyworm. Notably, compounds IIa, IIIa, IVa exhibited 100% activity at \(1\, \hbox {mg}\,\hbox {L}^{-1}\), in particular, IIa showed a comparable control efficacy to that of the commercial product flubendiamide. The SAR of these N-cyano sulfiliminyl isomers can be summarized as follows (Sc, Ss) \(\ge \) (Sc, Rs), while the N-trifluoroacetyl sulfiliminyl isomers is (Sc, Rs) \(\ge \) (Sc, Ss). Comparative molecular field analysis indicated that an electropositive substituent, \(\hbox {CH}_{3}\) group in the benzene ring was very important for the improvement in biological activity. These results could hold promise for novel chiral sulfiliminyl RyR regulators.     

Stereoselective aldol reactions of dihydroxyacetone derivatives catalyzed by chiral Zn2+ complexes

The direct aldol reaction between a protected dihydroxyacetone derivative and 4-nitrobenzaldehyde catalyzed by chiral Zn²⁺ complexes of 1-(n-carboxylalkyl)-7-aminoacyl-1,4,7,10-tetraazacyclododecane is reported. New Zn²⁺ complexes containing l-histidine and carboxylalkyl chains that mimic a class II aldolase, carboxypeptidase A and a serine protease were designed and synthesized. Syn-aldol products were mainly formed by an aldol reaction of acetonide-protected dihydroxyacetone with benzaldehydes and other benzaldehydes in N-methylpyrrolidone (NMP)/alcohol (MeOH, EtOH or 2-PrOH) in good yields with a high degree of diastereo- and enantioselectivity (56%～quant., 57～>99% ee). Mechanistic aspect based on ESI-HRMS, elemental analysis and pH titrations of model ligands is also discussed.