TurboFlow在线净化/液相色谱-串联质谱法快速测定动物源性食品中聚醚类抗生素的研究

建立了Turbo Flow在线净化/液相色谱-串联质谱法快速同时测定牛奶、鸡肉和鸡蛋中拉沙洛菌素、盐霉素、莫能菌素、甲基盐霉素、马杜霉素和尼日利亚菌素残留的方法。样品提取液经在线净化柱Cyclone-p净化,Thermo Scientific Hypersil-Gold C8(150 mm×2.1 mm,5μm)色谱柱分离,电喷雾正离子模式测定,整个分析过程仅13 min。方法在1~100μg/L范围内呈良好线性关系(r≥0.999),定量下限为1μg/kg,在动物源性食品中3个加标水平下的回收率为71.9%~109.0%,相对标准偏差为1.5%~14.9%。     

鱼组织中双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素含量的超高效液相色谱法测定

建立了黄颡鱼、团头鲂和草鱼血浆、肌肉、肝脏、肾脏中双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素同时测定的超高效液相色谱紫外检测法(UPLC-UV)。样品经乙腈(含0.01%乙酸)提取,无水硫酸钠除水,正己烷去脂等样品处理,在ACQUIT UPLC BEH C18色谱柱上分离,428 nm波长处测定。双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素在0.01~5.00 mg/L浓度范围内呈良好的线性关系,相关系数(r2)分别为0.998 7,0.999 8和0.999 6。在空白鱼组织中进行0.025,0.05,0.50,1.00 mg/kg 4个水平的加标回收实验,3种待测组分的平均回收率为64.7%~102.2%,相对标准偏差为0.69%~10.8%。鱼组织中3种待测组分的检出限(LOD)均为0.010 mg/kg,定量下限(LOQ)均为0.025 mg/kg。应用该方法研究了姜黄素在团头鲂体内的药代动力学规律。     

共沉淀法制备LiMn_xCo_yO_2的显微结构及其电化学性能

通过共沉淀法制备前驱体,随后在900℃下经不同时长烧结得到了层状LiMn_xCo_yO_2。X射线衍射、扫描电镜和透射电镜的研究结果表明,层状LiMn_xCo_yO_2的晶体结构是菱面体点阵,空间群是R3m,点阵常数与LiCoO_2非常接近。不同烧结时长下得到的样品在扫描电镜下均呈球状,随着烧结时间延长,球形规整度变得更好。对不同样品的电化学性能测试表明,烧结时间越长,样品中Mn的相对含量越高,其首次充放电比容量和循环性能越好。     

凹角区域双曲外问题的精确人工边界条件

研究一类凹角区域双曲型外问题的数值方法.先用Newmark方法对时间进行离散化,在每个时间步求解一个椭圆外问题.然后引入人工边界,并获得精确的人工边界条件.给出半离散化问题的变分问题,证明了变分问题的适定性,并给出了误差估计.最后给出数值例子,以示该方法的可行性与有效性.     

Sol-gel technique for the generation of europium-doped mesoporous and dense thin films: A luminescent study

In this paper, a series of europium-activated titania mesoporous and dense thin films were prepared by sol-gel process. Structural characterizations show that high europium ion loadings can be incorporated into titanium dioxide walls without destroying the mesoporous arrangement. However, high europium content locks the titanium dioxide crystallization process. Upon 10% europium ions loading, mesoporous thin films are mainly amorphous, whereas dense ones are still partially crystallized. Eu³⁺ ion luminescence has been investigated by exciting through the semiconductor host lattice. Emission features reveal that europium ions adopt similar environments (nanocrystalline and glassy-like ones) in both dense and mesoporous thin films. Fluctuations of europium emission under continuous UV excitation have been observed. One observes that the effect strongly depends on the thin films’ crystalline character which is strongly related with the texturation and existence at the mesoscopic length scale.     

Fuzzy Markov Chains and Decision-Making

Decision-making in an environment of uncertainty and imprecision for real-world problems is a complex task. In this paper it is introduced general finite state fuzzy Markov chains that have a finite convergence to a stationary (may be periodic) solution. The Cesaro average and the -potential for fuzzy Markov chains are defined, then it is shown that the relationship between them corresponds to the Blackwell formula in the classical theory of Markov decision processes. Furthermore, it is pointed out that recurrency does not necessarily imply ergodicity. However, if a fuzzy Markov chain is ergodic, then the rows of its ergodic projection equal the greatest eigen fuzzy set of the transition matrix. Then, the fuzzy Markov chain is shown to be a robust system with respect to small perturbations of the transition matrix, which is not the case for the classical probabilistic Markov chains. Fuzzy Markov decision processes are finally introduced and discussed.     

Necessary contact conditions for charge injection development into KBr single crystals

We have studied the current vs time behaviour of KBr single crystals by applying a constant voltage between a pointed cathode and a flat anode at constant temperature. The obtained curves are characterized by three or four different zones. We report here very detailed results on the first one. We conclude that in this zone the current through the crystal is purely ionic. As a consequence of this ionic transport, K atoms accumulate at the pointed cathode to form a new electrode. This acts as an injecting contact for electronic current. Electron injection currents and, therefore, colour center clouds that developed upon the formation of this new injecting contact, mark the start of zone II of the current vs time curve. Simple equations are proposed to explain the kinetics of zone I. Experiments by other authors are also analyzed. Finally, a discussion on the simpler experimental conditions required to create the new injecting contact is presented. Results on zones II and III will be published in the near future.     

Analytical properties of 2-oximinodimedone dithiosemicarbazone

The synthesis and analytical properties of 2-oximinodimedone dithiosemicarbazone are described.     

Non-aqueous fluorimetric determination of scandium in silicate rocks

A method for the fluorimetric determination of scandium with 1,2,7-trihydroxyanthraquinone in dimethylformamide medium is described. The calibration graphs obtained by the normal, synchronous, and synchronous first and second derivative techniques are linear between 12 and 225 ng/ml, and the detection limit is 2 ng/ml. The method is applied to the determination of Sc(III) in two simulated and two naturally occurring rocks.     

Mise en evidence de la chiralité de l'édifice spirophosphoranique

The chirality of the spirophosphorance skeleton of the recemic mixture 2a , 2ā , is revealed by the NMR chiral shift reagent.