反相离子对液相色谱法测定欧洲鳗鲡体中丙硫咪唑及其代谢物的残留量

建立了鳗鲡体中丙硫咪唑及其代谢物残留量测定方法。样品用乙腈提取,经正己烷净化后,液相色谱一荧光法测定,标准加入法定量。流动相为：甲醇、乙腈和乙酸铵,梯度洗脱。检测波长为：激发波长290nm,发射波长320nm,丙硫咪唑、2氨基丙硫咪唑砜、丙硫咪唑亚砜、丙硫咪唑砜检出限依次为：25、5、10、1μg／kg。回收率大于95％,相对标准偏差小于8％。     

3-乙氧基-4-羟基苯乙醇酸在聚邻甲苯胺-Cu~(2+)膜电极上的电氧化

采用循环伏安法制备了聚邻甲苯胺(POT)膜电极,再以浸泡吸附法在此膜中嵌入Cu2+,制成POT-Cu2+膜电极.研究了POT-Cu2+膜电极对3-乙氧基-4-羟基苯乙醇酸的电氧化行为,并讨论了影响电氧化活性的主要因素.结果表明,50℃下,在含有0.5mol.L-13-乙氧基-4-羟基苯乙醇酸的1.5mol.L-1氢氧化钠溶液中,POT-Cu2+膜电极具有高的电氧化活性和良好的稳定性.将该电极用于3-乙氧基-4-羟基苯乙醇酸电解氧化脱羧制备乙基香兰素,在0.55V(vsSCE)下恒电位电解1h,乙基香兰素的产率可达89%以上,电流效率达97%以上.     

黑蚂蚁的脂肪酸及抗氧化性能的分析

对黑蚂蚁中脂肪酸的组成和含量进行测定。采用索氏提取法提取其脂肪酸,再进行甲酯化处理,以气相色谱-质谱联用仪进行了分离和鉴定。由黑蚂蚁中分离鉴定出11种脂肪酸,占脂肪酸总量的99.78%,不饱和脂肪酸占脂肪酸总量的80.65%,饱和脂肪酸占脂肪酸总量的19.13。通过流动注射化学发光法分析了黑蚂蚁的抗氧化性能,结果表明,黑蚂蚁具有较强的抗氧化性能。     

Separation,identification, and structural characterization of sucrose ester isomers from tobacco

Sucrose esters (SEs) are crucial tobacco smoke flavor precursors and play a significant role in tobacco's functionality. Due to their structural complexity, the separation and analysis of SEs in tobacco remain a major challenge, and massive structures of SEs have not yet been fully identified. In this study, the fractions enriched in SEs were obtained from oriental and flue-cured tobacco through a series of pretreatments, and two types of SEs (Types I and II) were distinguished by liquid chromatography-tandem mass spectrometry (LC-MSⁿ) analysis, with Type II SEs newly characterized in tobacco. Five groups of main SEs were further purified using preparative high-performance LC (HPLC) coupled to an evaporative light scattering detector, and their structures were characterized by nuclear magnetic resonance spectrometry techniques including ¹H, ¹³C, correlation spectroscopy, heteronuclear single quantum correlation, and heteronuclear multiple bond correlation. By combining LC-MSⁿ and nuclear magnetic resonance spectrometry, the structures of eight SE isomers were finally proposed, of which four were newly identified. These findings further enhance the understanding of the structural diversity of SEs in tobacco, serving as a valuable reference for future research on the elucidation, synthesis, and metabolism of SEs.     

Residue and dissipation of zinc thiazole in tobacco field ecosystem

A high-performance liquid chromatography with ultraviolet (HPLC-UV) detection method after derivatisation was developed for the first time for the novel fungicide zinc thiazole residue in tobacco samples. Field trials in two different locations were conducted to investigate the dissipation and residue of zinc thiazole in tobacco leaves and soil. The average recoveries of zinc thiazole were in the range of 82.5%–93.9% with relative standard deviations (RSDs) of 1.2%–9.1%. The zinc thiazole showed a rapid dissipation rate in fresh tobacco leaves with the half-lives of 1.1–1.6 days. The terminal residues of zinc thiazole in cured tobacco leaves and soil were 2.8–28.0 mg kg^?1and <0.05 mg kg^?1, respectively. The results could be used to establish the maximum residue limits (MRLs) and provide guidance for the scientific use of zinc thiazole in agriculture.     

液固反应微观-宏观关联模型及实验验证

当液一固反应为流体扩散控制时,以缩核模型为基础,得到了单颗粒消溶时粒径的变化规律,满足平方反比定律;在单颗粒消溶的基础上,建立了颗粒群消溶模型,得到了单颗粒微观反应模型和颗粒群宏观反应特征的关联关系.以不同种类的石灰石在不同温度和pH值下的消溶过程为例,对液固反应的微观-宏观关联模型进行了实验验证,实验和数学模型吻合较好.该关联模型对完善液固反应理论体系,实现宏观实验数据反推微观化学反应参数的测量技术具有重要意义.     

Nanoscale Thermal Response in ZnO Varistors by Atomic Force Microscopy

We report the application of customer-built scanning thermal microscopy （SThM） based on a commercial atomic force microscope to investigate local thermal inhomogeneity of ZnO varistors. The so-called 3ω method, generally used for measuring macroscale thermal conductivity, is set up and integrated with an atomic force microscope to probe the nanoseale thermal property. Remarkably, thermal contrasts of ZnO varistors are firstly imaged by the SThM, indicating the uniform distribution of spinel phases at triple points. The frequency-dependent thermal signal of ZnO varistors is also studied to present quantitative evaluation of local thermal conductivity of the sample.     

棉籽化学成分的分析

采用索氏提取法对棉籽中棉籽油进行了提取,以气相色谱-质谱联用仪进行了分析,分离鉴定出10种脂肪酸,占棉籽油总量的99.52%。并对其主要成分进行了鉴定,主要化学成分为:棕榈酸26.68%,亚油酸66.05%。用蒸馏-萃取法提取棉花籽中挥发性物质,测得棉籽挥发油的量为0.80%,用GC/MS法从棉籽挥发油中分离并确定出16种化学成分。用峰面积归一化法通过化学工作站数据处理系统,得出各化学成分在挥发油中的质量分数。其中主要成分为:石竹烯量高达33.27%。     

燃料爆炸抛撒过程中射流量的估算

通过高速录像记录3种质量不同、长径比为1.5~2.3的燃料空气炸药（FAE）装置爆炸抛撒过程的实时结果,用专门的软件对图像进行了处理。以装置上端盖为基准对解体时间进行了初步估算,由此给出了燃料初期射流量的理论估算式,结合试验结果计算了燃料的射流量。结果表明,燃料的射流量与装置的高度、装置的材质和燃料的密度等因素有关,实验研究的3种装置射流量均大于总燃料量的10%。     

DERIVATIVES OF EIGENPAIRS OF SYMMETRIC QUADRATIC EIGENVALUE PROBLEM

Derivatives of eigenvalues and eigenvectors with respect to parameters in symmetric quadratic eigenvalue problem are studied. The first and second order derivatives of eigenpairs are given. The derivatives are calculated in terms of the eigenvalues and eigenvectors of the quadratic eigenvalue problem, and the use of state space representation is avoided, hence the cost of computation is greatly reduced. The efficiency of the presented method is demonstrated by considering a spring-mass-damper system.