Flow-injection spectrophotometric determination of sulfadiazine and sulfamethoxazole in pharmaceuticals and urine.

A rapid and sensitive flow-injection spectrophotometric method is proposed for the determination of sulfadiazine and sulfamethoxazole. This method is based on the diazotization of sulfonamide with sodium nitrite, and a coupling reaction of the diazo-compound with alpha-naphthylamine. The optimum experimental conditions are obtained by using the controlled and weighted centroid simplex method. The linear ranges for the determination of sulfadiazine and sulfamethoxazole are 0.2-20 microg ml(-1) and 0.1-20 microg ml(-1), and their detection limits are 0.06 microg ml(-1) and 0.05 microg ml(-1), respectively, and the sampling frequency is 130 samples per hour. The method has been used to determine sulfadiazine and sulfamethoxazole in pharmaceuticals and urine without separation. The results are in agreement with those obtained by a high-performance liquid chromatograph technique at the 95% confidence level.     

FFC-1离子交换纤维对酸碱有害气体吸附性能的研究

系统考察了不同直径及反离子形式的FFC-1聚羧酸离子交换纤维对酸碱有害气体的穿透吸附,各种温、湿度条件下的吸水率,以及作为有害气体吸附滤除材料的重复使用与再生性能。研究表明:FFC-1纤维直径的减小有利于提高对有害气体的动态吸附容量。在体系温度、相对湿度分别为15℃、50%时,以3D腈纶为起始原料的钠型FFC-1离子交换纤维的吸水率≥350mg/g.纤维;对SO2的穿透吸附容量可达200mg/g.纤维。FFC-1离子交换纤维具有良好的重复使用与再生能力,经20次再生循环使用后,纤维交换容量未见明显变化。     

四元缔合物体系薄层树脂相分离与光度法联用测定痕量钴

提出了在酸性条件下 (pH=5.0),利用阳离子交换树脂-丁二酮肟-碘-钴四元体系,通过薄层树脂相光度法测定钴的新方法。本法灵敏度高 (e454=1.7105L/molcm),比水相光度法提高14倍,精密度理想 (测定2.0礸/ml Co(II) 6次,RSD=1.3%),选择性好。实测药品VB12及天然水中钴,线性范围0.024~2.0礸/ml (定容50ml),检出限10.4ng/ml。     

Asymmetric palladium-catalyzed benzylic nucleophilic substitution: high enantioselectivity with the DUPHOS family ligands

The asymmetric palladium-catalyzed benzylic reaction of 1-(2-naphthyl)ethyl acetate and its 6-methoxy substituted analogue with dimethyl malonate anion led to substitution products with up to 90% ee when the iPr-DUPHOS chiral ligand was used.     

Growth control of homogeneous pulsed electrodeposited Co thin films on n-doped Si(1 1 1) substrates

Cobalt thin films were deposited by pulsed electrodeposition on n-doped silicon substrates. We show that the morphology and the magnetic properties of the samples can be controlled by a careful choice of the deposition conditions. Atomic force microscopy measurements reveal a granular growth with grain size and homogeneity strongly dependent on the total deposition time and pulse frequency of the applied signal. Magnetic force microscopy and magnetization measurements indicate the formation of magnetically correlated grain systems with a maximum magnetic correlation and homogeneity for samples with grain diameters of about 40 nm.     

Review of absolute doubly differential cross-section experiments and cross-section ratios for electron bremsstrahlung from rare gas atom and thin-film targets

We discuss doubly differential cross-section experiments for electron bremsstrahlung from free gas atom and thin-film targets for electron energies of 100 keV or less. We compare cross-section ratios for different target atoms with two theoretical models: ordinary bremsstrahlung and total bremsstrahlung calculated in the stripping approximation. Ratios of cross sections have been used to improve the comparison between experiment and theory when only relative cross sections are available or when the error in the absolute cross section is large. We also discuss additional background processes that may be more important in gas target experiments.     

The dynamic kinetic resolution of 3-oxo-4-phenyl-β-lactam by recombinant E. coli overexpressing yeast reductase Ara1p

Using a recombinant E. coli strain overexpressing yeast reductase Ara1p, we reduced racemic 3-oxo-4-phenyl-β-lactam to cis-(3S,4R)-3-hydroxy-4-phenyl-β-lactam as a single enantiopure product. The dynamic kinetic resolution occurred over the course of fermentation at pH 7. Under the same conditions, 3-oxo-4-(2-thiophenyl)-β-lactam 4 and 3-oxo-4-(2-furyl)-β-lactam 5 were not resolved.     

Synthesis and X-ray crystal structure of oxamido-bridged heterobinuclear Ni(Ⅱ)-Cu(Ⅱ) complexes

The two complexes [Ni(oxen)Cu(L)2](ClO4)2.xH2O (L=2,2'-bipyridyl(bpy), 1,10-phenanthroline(phen)) have been synthesized, where oxen is N,N'-bis(2-aminoethyl)oxamido di-anion. The crystal structure of [Ni(oxen)Cu(bpy)2](ClO4)2.CH3OH has been determined by X-ray diffraction method. The crystal is triclinic system, space group P1 with a=12.179(1),b=12.298(2), c=11.476(2) A, a=97.57(1), B=97.52(1), 7=80.29(2), V=1669.04(67) A3, Z=2, Dcalcd=1.667 g/cm3. The structure has been refined to final R of 0.076 and Rw of 0.080, respectively. The complexes have an extended oxamido-bridged structure and consist of Ni(Ⅱ) ion in a square planar environment and Cu(Ⅱ) ion in a distorted octahedral environment.     

A new trend in the synergistic extraction of rare-earth(III) complexes with various β-diketones and 1,10-phenanthroline

The synergistic extraction of rare-earth (RE) [La(III), Sm(III), Tb(III) and Lu(III)] complexes, with three β-diketones (HA) [hexafluoroacetylacetone (Hhfa), pivaloyl-trifluoroacetone (Hpta) and benzoylacetone] in the presence of a bidentate ligand (S), 1,10-phenanthroline, in benzene was investigated. The general composition of the adducts formed is expressed as RE(A)₃S. RE(A)₃(S)₂ is also observed in La-Hhfa, La-Hpta and Sm-Hhfa systems. The adduct formation contains β_s,1 and β_s,2 and the synergistic extraction constants K_ex,s,1 were determined. The trend of these constants is discussed in terms of the RE(III), β-diketone, neutral bidentate ligand and organic solvent.     

无机元素与计量学模型结合的半夏产地溯源研究

目的:建立不同产地半夏无机元素的分析方法和溯源体系,为半夏药材的质量控制和道地性评价提供技术支持。方法:采用电感耦合等离子体质谱法(ICP-MS)和电感耦合等离子体原子发射光谱法(ICP-AES)对我国6个主产区72份半夏样品中K、Ca、Na、Mg、Al等37种无机元素的含量进行测定,并采用方差分析、主成分分析、因子分析等计量学方法进行统计与评价。通过对比BP-神经网络算法、K-最近邻算法、最小二乘支持向量机等多种模式识别方法,探索适合半夏产地溯源的最佳模型。结果:不同产地半夏中无机元素的构成各具特征,各无机元素含量在产地间差异显著(P＜0.05),其中La、Pb、As、Na、Bi、Hg、Sn、Cd、Ag 9种元素在不同产区间的差异最为明显;3D-plots图显示不同产地半夏样品分布相对集中,具备产地分类的可行性;KNN分类模型(曼哈顿距离)是半夏产地溯源的最佳方法,测试集的正确率达到100%。结论:无机元素分析技术结合适当的计量学模型可以实现半夏的产地溯源。