Simultaneous determination of residual antiparasitic lactones in bovine muscle and liver by liquid chromatography with fluorescence detection

Abamectin, doramectin, eprinomectin, ivermectin, milbemectin, and moxidectin in bovine muscle and liver were extracted with acetonitrile. The extracts were partitioned with n-hexane and then evaporated to dryness. The residue was cleaned up on Bond Elute NH2 cartridge, and the drugs were eluted from the cartridge with methanol-ethyl acetate (3 + 7). The eluate was evaporated to dryness, and residues were derivatized with N,N-dimethylformamide-acetic anhyride-1-methylimidazole. The derivatives were determined by liquid chromatography with fluorescence detection. Recoveries of the 6 drugs were 79.6-63.8% in muscle and 71.6-60.6% in liver at 0.01 ppm levels. The quantitation limits were 5 ppb for each drug.     

CdTe量子点DNA荧光纳米探针的合成及表征

采用水相合成法合成了巯基乙酸(TGA)修饰的水溶性CdTe量子点,通过反相微乳液法制备了二氧化硅及壳聚糖修饰的核壳型复合荧光纳米粒子,将其与DNA吸附连接,得到CdTe量子点DNA荧光纳米探针。用扫描电镜、透射电镜、荧光光谱、红外光谱、紫外光谱、ζ电位等测试方法对产物的理化性质进行了分析表征。结果表明制备了表面富含氨基的复合荧光纳米粒子,其对DNA具有良好的吸附作用。     

Synthesis,characterization, thermal properties,and antimicrobial activity of 4‐chloro‐3‐methyl phenyl methacrylate/8‐quinolinyl methacrylate copolymers

4‐Chloro‐3‐methyl phenyl methacrylate (CMPM) and 8‐quinolinyl methacrylate (8‐QMA) were synthesized through the reaction of 4‐chloro‐3‐methyl phenol and 8‐hydroxy quinoline, respectively, with methacryloyl chloride. The homopolymers and copolymers were prepared by free‐radical polymerization with azobisisobutyronitrile as the initiator at 70 °C. Copolymers of CMPM and 8‐QMA of different compositions were prepared. The monomers were characterized with IR spectroscopy and ¹H NMR techniques. The copolymers were characterized with IR spectroscopy. UV spectroscopy was used to obtain the compositions of the copolymers. The monomer reactivity ratios were calculated with the Fineman–Ross method. The molecular weights and polydispersity values of the copolymers were determined with gel permeation chromatography. The thermal stability of the polymers was evaluated with thermogravimetric analysis under a nitrogen atmosphere. The homopolymers and copolymers were tested for their antimicrobial activity againstbacteria, fungi, and yeast. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 157–167, 2005     

Reaction of Lithium Cellulosate with Episulfides

The reactions of propylene, ethylene, and styrene sulfide with cotton fabrics in the form of their lithium cellulosate derivative, obtained by metallation with lithium methoxide, were studied. Both graft and homo-polymerization took place and in the reaction with propylene and ethylene sulfide, cotton fabrics with high polysulfide content were obtained. With propylene sulfide 50% of the monomer polymerized was grafted. The effects of monomer concentration, cellulosate degree of substitution, reaction time, and solvent on the polymerization were investigated. In contrast with propylene and ethylene sulfide, only small conversions were obtained in the reaction with styrene sulfide. The results were attributed to steric effects.     

Effect of solvents on the electrochemistry of olefins and aromatic molecules

Cyclic voltammetry and electrolysis studies were carried out in dimethyl sulfoxide, diglyme and liquid ammonia. The depolarizers were diethyl fumarate, ethyl cinnamate, stilbene and anthracene. The reduction reactions were carried out in the presence of organic halides, phenol, acids and water. The rates of the reactions were measured. The main solvent effect was noticed with water which reacts 100 times faster in diglyme than in liquid ammonia or DMSO. The results of electrolytic experiments with two reactants simultaneously were compared with those predicted from the kinetic data.     

在线固相萃取净化-液相色谱-串联质谱法测定猪肉中10种大环内酯类抗生素

建立了在线固相萃取净化-液相色谱-串联质谱检测猪肉中10种大环内酯类抗生素残留的方法。样品经过乙腈提取,提取液40℃旋蒸至干后,分析物用2 mL磷酸盐缓冲液溶解,溶解液经在线固相萃取柱(HLB柱)富集净化,甲醇洗脱,然后转移至XBridge BEH C18色谱柱上,以10 mmol/L乙酸铵水溶液和乙腈溶液为流动相进行分离,最后用串联四极杆质谱检测。结果表明,10种大环内酯类抗生素在0.1~200μg/L范围内呈现良好的线性关系,相关系数均大于0.990。方法的检出限范围为0.05~0.30μg/kg,定量限范围为0.10~1.00μg/kg;添加水平为0.10~10.0μg/kg时,方法回收率为69.6%~115.2%,相对标准偏差(RSD)10%。该方法可以作为猪肉中大环内酯类抗生素的检测方法。     

气相色谱-质谱法同时测定聚氯乙烯塑料制品中的10种有机锡化合物

采用气相色谱-质谱法(GC-MS)同时快速有效地测定了聚氯乙烯（PVC）塑料制品中的二丁基氯化锡、单丁基氯化锡、三乙基氯化锡、三苯基氯化锡、三丁基氯化锡、三丙基氯化锡、二苯基氯化锡、四丁基锡、二辛基氯化锡和单苯基氯化锡等10种有机锡化合物。使用四氢呋喃溶解PVC样品,甲醇沉淀样品中的聚合物,超声萃取其中的有机锡化合物,将提取液衍生化后用正己烷萃取,采用GC-MS总离子流和选择离子进行定性定量测定。对衍生化时间、衍生化pH值、衍生化试剂用量、沉淀试剂用量等样品前处理条件进行了优化,并进行了线性关系、回收率、精密度等考察。结果表明,方法的线性范围为0.5～50 mg/L,线性相关系数为0.9978～0.9997。10种有机锡化合物的回收率及相对标准偏差(n=9)分别为84.23%～109.1%和4.24%～10.75%。所建立的方法能很好地应用于PVC塑料制品中有机锡化合物的检测。     

液液分散微萃取/GC-MS法测定婴幼儿一次性用品中5种致敏原物质

建立了同时测定婴幼儿一次性用品中5种致敏原物质(柠檬烯、沉香醇、柠檬醛、乙酸苄酯和肉桂醛)的分散液液微萃取/气相色谱-质谱(DLLME/GC-MS)检测方法。样品经乙腈浸泡提取、水分散和盐析后用四氯化碳萃取浓缩,采用GC-MS测定,外标法定量。目标物在0.01~10 mg/kg范围内线性关系良好,相关系数在0.99以上。方法检出限为0.01~0.1 mg/kg。加标回收率为78.7%~106%,相对标准偏差为2.4%~11.3%。该方法前处理简单,灵敏度高,可满足纸尿裤、婴儿专用湿巾等一次性婴幼儿用品中5种致敏原物质的检测要求。     

Synthesis and photochemistry of side-chain liquid crystal polymers based on cinnamate esters

The syntheses of three methacrylate monomers with cinnamate ester side-chains and of a further monomer with a corresponding cinnamide side-chain are described. Two of the monomers, with isomeric structures, were thermotropic liquid crystals. Although the clearing points were very similar the crystal melting points differed by 8°C. One compound also exhibited a monotropic smectic phase, behavior not shown by its isomer. The other two monomers were not liquid crystalline. The monomers were polymerized by free radical polymerization, both as homopolymers and as copolymers with methyl methacrylate. In the case of one of the mesogenic ester monomers, copolymers with a cyanophenyl benzoate monomer were also prepared. Three of the four monomers formed thermotropic liquid crystalline homopolymers and the copolymers with the benzoate monomer were also liquid crystalline. The monomers were considered as photoactive components of polymeric liquid crystals. As a preliminary investigation of their photochemistry, copolymers with methyl methacrylate were prepared and irradiated in solution with a broad-band source. Under these conditions two of the materials show a facile photo-Fries rearrangement of the aryl cinnamate ester group. © 1992 John Wiley & Sons, Inc.     

Copper(II) complexation with 1-methyl-2-mercaptoimidazole in 7 M HCl

The complexation of copper(II) with 1-methyl-2-mercaptoimidazole in 7 M HCl was potentiometrically studied. The compositions of complexes were determined, and their stepwise formation constants were calculated. The complexes were shown to become less stable with increasing temperature. The thermodynamic functions of complexation were estimated. The copper complexes were shown to surpass the rhenium complexes in stability.     

电感耦合等离子体原子发射光谱法(ICP-AES)测定高效复合孕育剂中铝、钙、钡

通过硝酸、氢氟酸和盐酸分解试料,高氯酸冒烟驱走硅和氟,最后用盐酸溶解盐类,应用电感耦合等离子体原子发射光谱法(ICP-AES)对高效复合孕育剂中铝、钙、钡进行测定,方法能准确、快速地测定其含量,加标回收率在98.8%~103%,精密度、标准样品分析对照均取得了满意的结果。     

The thermodynamic characteristics of formation of Zn<Superscript>2+</Superscript> complexes with D,L-tryptophan in aqueous solution

The heat effects of formation of D,L-tryptophan complexes with doubly charged zinc ions were determined calorimetrically. The heat effects of interaction of amino acid solutions with a solution of Zn(II) were measured at 288.15, 298.15, and 308.15 K and ionic strengths of 0.25, 0.50, and 0.75 against the background of KNO₃. The heats of dilution of solutions of zinc nitrate with solutions of the background electrolyte were determined under the same conditions. The corresponding corrections were introduced. The thermochemical data were processed taking into account step equilibria. Along with complex formation, “side” protolytic processes were included. The standard thermodynamic characteristics of complex formation were calculated. The influence of temperature on the heat effects of complex formation in the β-alanine-zinc(II) ions system was considered.     

Synthesis,characterization, and antimicrobial activity of some novel poly(ether ketone)s

Low molecular weight poly(ether ketone)s were synthesized from phenol, 1,4‐phenylenedioxy diacetylchloride, chloroacetylchloride, and dichloroalkanes [1,2‐dichloroethane and dichloromethane] by a Friedel–Crafts reaction with anhydrous aluminum chloride as a catalyst and carbon disulfide as a solvent. The conditions for the preparation of the poly(ether ketone)s and the chlorine contents obtained with the Carius method were examined, and a reaction scheme for each resin was established. The molecular weights and polydispersities of the resins were obtained by gel permeation chromatography. The polyketones were characterized by IR spectroscopy. The characteristic frequencies due to different functional groups were assigned. The thermal properties of the resins were studied with thermogravimetry and differential scanning calorimetry. The characteristic temperatures of thermal degradation for the poly(ether ketone)s were evaluated with thermogravimetric analysis. The kinetic parameters for the decomposition reactions of the resins were obtained with Broido and Doyle's method, and the heats of fusion were obtained from differential scanning calorimetry thermograms. The polyketones were thermally stable up to 200 °C. All the polyketones were tested for their microbial properties against bacteria, fungi, and yeast. The effect of poly(ether ketone)s on the growth of these microorganisms was investigated, and the polyketones were found to inhibit the growth of the microorganisms to a considerable extent. © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 2335–2344, 2003     

Spectroscopic,structure, and DFT studies of cationic palladium(II) complexes with imidazole derivative ligands

Two palladium(II) complexes with imidazole derivative ligands have been synthesized. The molecular structures of the complexes were determined by X-ray crystallography and their spectroscopic properties were studied. Based on the crystal structures, computational investigations were carried out to determine the electronic structures of the complexes. The electronic spectra were calculated with use of time-dependent DFT method, and the transitions were correlated with the molecular orbitals of the complexes. The emission of the complex with 1-methylimidazole was examined.     

Identification of metabolites of the anabolic steroid methandienone formed by bovine hepatocytes in vitro.

Monolayer cultures of bovine hepatocytes were used to investigate the biotransformation of methandienone in vitro. After incubation of bovine hepatocytes with methandienone, samples were taken at different times. The samples were treated with deconjugation enzymes and extracted with diethyl ether. The metabolites formed were converted to their trimethylsilylether derivatives. By using gas chromatography-mass spectrometry with electron impact and chemical ionisation, several metabolites were identified. After 24 h of incubation with bovine hepatocytes, 83% of the parent compound was converted to its metabolites. The major metabolite found was 6-beta-hydroxymethandienone with a yield of 24%. This compound was identified after comparison with an authentic sample of 6 beta-hydroxymethandienone, which was synthesized chemically.     

Boron analysis in biological material: microwave digestion procedure and determination by different methods

Investigations were made on the determination of boron in biological material. A procedure using the microwave digestion technique was optimised. The analyses were performed by photometry with azomethine-H, fluorimetry with carminic acid, inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry. The matrix interferences, the interferences caused by iron and the detection limits were investigated for these methods. Determinations were performed for plant material, wheat, milk, meat and blood plasma. Recoveries and precision of all methods were studied. To test accuracy and precision, four NBS reference materials were analysed and the results compared with the values in literature. Good recoveries were found with all methods, except the fluorimetric technique. The boron content found in the NBS standard reference materials agreed well with data reported before. Best precision was obtained for the two ICP methods. The azomethine-H method gave good results when material of high boron content was analysed. With the carminic acid method no reliable results were achieved.     

大鼠海马三维结构及学习记忆能力在连续缺碘子代的表现

用低碘饲料复制了连续多代的大鼠克汀病模型，研究了第１代和第２代子鼠的学习记忆能力和重建的海马三维结构。结果表明，与正常组大鼠比较，克汀病子鼠生长发育迟缓，甲状腺呈增生性甲状腺肿病变，其血清甲状腺激素水平降低，逃避防御条件反射显示学习记忆能力低下等。以上病在第二代克汀鼠明显重于第一代。海马结构损害是克汀病大鼠学习记忆能力低下的形态学基础。     

Equilibrium analysis of reactions of metal-pyridylazoresorcinolato chelates with quaternary ammonium ion, nonionic surfactant and polyethylene glycol in aqueous solution by capillary zone electrophoresis.

The resolutions of metal-4-(2-pyridylazo)resorcinol chelates by capillary zone electrophoresis (CZE) were investigated in the presence of some interacting reagents; also, equilibrium reactions between the chelates and the interacting reagents were analyzed in an aqueous solution. Among nine metal chelates formed in aqueous solution, the chelates of VV, FeII, CoIII, NiII, and CuII were resolved and detected by CZE, while other chelates were decomposed during electrophoretic migration. The electrophoretic mobility of the chelates of FeII, NiII, and CuII increased with increasing pH of the migrating solution; also, the acid-dissociation constants of these three chelates were determined by analyzing the mobility change. The ion-association constants of the five anionic chelates and pyridylazoresorcinolate ion with quaternary ammonium ions were also determined by analyzing the mobility change. The binding behavior of the ligand and its chelates with nonionic surfactant micelle, as well as with polyethylene glycol, were investigated, and their binding constants were determined through the mobility change. When Brij 35 was used as a nonionic surfactant interacting with the anionic chelates, the FeII chelate decomposed at Brij 35 concentrations over 6.67 mM. The equilibrium constants and the reactivity were compared with each other.     

稀土(III)-冠醚配位反应的热力学性质: II. 镧系(III)高氯酸 盐与二苯并18- 冠-6在无水乙腈中配位反应的量热滴定研究

用滴定量热计于298.15K测定了除钷、镥以外的全部十三种镧系(III)高氯酸盐与二苯并-18-冠-6在无水乙腈中的配位作用。借助计算机用自编程序算出了配位反应的生成常数和焓变,进而算出了配位反应的自由能变化和熵变化。探讨了镧系(III)阳离子对配位反应的影响。此外,还比较了几种不同冠醚与高氯酸镧在无水乙腈中配位反应的热力学性质。