LC-MS/MS定量测定大鼠和人肝微粒体孵育液中丁苯酞浓度方法的建立

正丁苯酞(n-butylphthalide,NBP),又名芹菜甲素,是我国心脑血管领域第一个拥有自主知识产权的药物,它具有很强的抗脑缺血损伤作用,而毒副作用较低[1-2].     

水/油型微乳液中球形及棒状钛酸锶钡纳米粒子的控制合成

Barium strontium titanate nanoparticles with spherical and rod-like morphologies were synthesized in water/Triton X-100/n-hexanol/cyclohexane quaternary reverse microemulsion solution. The influences of the molar ratio of water to surfactant (ω₀) and the concentration of reactants on the morphology and size of barium strontium titanate nanoparticles were studied. The structure, compositions and morphology of the prepared products were characterized by XRD, SAED, ICP, EDS and TEM. The results show that the obtained Ba_0.7Sr_0.3TiO₃ spherical nanoparticles with diameters of 20～100 nm and the Ba_0.7Sr_0.3TiO₃ nanorods with diameters of 70～120 nm and lengths up to 600～800 nm are a single crystal, with a cubic phase. The molar ratio for barium, strontium and titanate in products is about 0.7:0.3:1.     

Hydrothermal Synthesis and Structural Characterization of a Novel Organic—Inorganic Hybrid Compound {[Cu（2,2′—bpy）2]2—Mo8O26}

A novel organic-inorganic hybrid compound {[Cu(2,2′-bpy)2]2Mo8O26} has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group, Pna21,with a=2.4164(5),b=1.8281(4),c=1.1877(2)nm,V=5.247(2)nm^3,Z=4,and final R1=0.0331,wR2=0.0727.The structure consists of discrete {[Cu(2,2′-bpy)2]2Mo8O26} clusters,constructed from a β-octamolybdate subunit[Mo8O26]^4- covalently bonded to two [Cu(2,2′-bpy)2]^2 coordination complex cations via bridging oxo groups.In addition,the spectroscopic properties and thernal behavior of this compound have been investigated by spectroscopic techniques (UV-vis,IR,Raman and EPR spectra) and TG analysis.     

S-甘油醛缩丙酮的合成及其Wittig反应

以L-抗坏血酸为原料合成了S-甘油醛缩丙酮;研究了S-甘油醛缩丙酮的Wittig反应立体选择性.     

2,4,6-三硝基苯酚改性锆铝复合氧化物固定相分离富勒烯的色谱性能研究

制备了用于分离C60和C70的2，4，6－三硝基苯酚改性锆铝复合氧化物高效液相色谱固定相，考察了流动相中甲苯的含量、柱温及流速对C60和C70分离的影响，同时比较了酸腐蚀前后锆铝复合氧化物基质对分离的影响，结果表明，2，4，6－三硝基苯酚改性酸腐蚀后锆铝复合氧化物填料对富勒烯表现出较强的分离能力，具有作为富勒烯制备分离的潜力。     

反复呼吸道感染儿童血锌检测分析

为探讨低锌对儿童反复呼吸道感染的影响 ,检测了 1 2 3例儿童指血锌 (Zn)值 ,并采用t检验 ,与正常儿童组进行血锌值比较。结果表明 ,反复呼吸道感染组血Zn值 48 69± 4 89μmol/L ,正常儿童组血Zn值 5 7 46± 1 9 1 8μmol/L ,经t检验 ,t>t0 0 1( 12 1) ,P <0 0 1 ,具有极其显著差异。提示儿童锌缺乏明显导致儿童免疫力下降 ,削弱机体对病毒及细菌的抵抗力 ,适当补锌有助于预防和治疗上呼吸道感染     

Organic Reactions in Ionic Liquids： An Efficient Method for the Synthesis of Phenacyl Esters by Reaction of Carboxylic Acids with α-Bromoacetophenone Promoted by Potassium Fluoride

An efficient method is reported for the synthesis of phenacyl esters by reaction of carboxylic acids with a-bromoacetophenone promoted by potassium fluoride in ionic liquid [Bmim]PF6, the yield of the reaction is almost quantitative and the products are essentially pure.     

2-氰基-3-甲硫基-3-取代甲氨基丙烯酸酯类化合物的合成及其除草活性

A series of 2-cyano-3-methylthio-3-substituted methylaminoacrylates were synthesized as herbicidal inhibitors of photosystem Ⅱ （PSⅡ） electron transport, in order to estimate the effect of fluorine atom, pyridyl group, chirality and ester chain on activity. The important intermediate 2-fluoro-5-aminomethylpyridine was synthesized with high yield. The bioassay results showed that most of rifle compounds had high herbicidal activity in postemergence treatment. The introduction of an a-methyl into the 3-substituted methylamino could improve the activity notably. The replacement of hydrogen by chlorine or fluorine group and phenyl by pyridyl group showed different effects, and at the same time, the ester chain affected the activity too.     

液相色谱-串联质谱法检测雄蜂蛹粉中50种抗生素残留

建立了液相色谱-串联质谱检测雄蜂蛹粉中50种抗生素残留（大环内酯类、喹诺酮类、磺胺类、四环素类、硝基咪唑类、林可霉素和氯霉素）的方法。样品经高氯酸溶液和醋酸铅溶液提取沉淀蛋白质，清液用磷酸氢二钾溶液调节pH值至8，经固相萃取净化后进行仪器分析。采用多反应监测正离子或负离子模式检测，可以一次完成对雄蜂蛹粉中50种目标化合物的定性和定量测定。50种抗生素的加标回收率为70.2%~118.3%，相对标准偏差（RSD）为1.8%~13.6%。该方法操作简便，灵敏度高，适用于雄蜂蛹粉中多种兽药残留的分析确证。     

手性试剂TMPEA用于手性酮对映体纯度测定的研究

β-三氟甲基-β甲氧基β-苯基乙胺（TMPEA）是含氨基功能团的手性试剂[1]．由于胺可将按酸转变成酸胺，该试剂已成功地用于手性有机酸对映体的纯度测定[2]．考虑到胺同样可将醛酮转变成亚胺，本文进一步探讨了TMPEA用于手性醒酮对映体纯度测定的可行性．用R－（－）－TMPEA及dl－TMPAE分别与下列4种手性酮反应，制备相应的非对映异构亚胶：比较光活亚胺及相应的非对映异构体混合物亚腔的NMR谱，可确定各组非对映异构亚胺‘HNMR位移差（以OCH为探针基团）和’‘FNMR的位移差（以CF为探针基团）（表1）．TablelCheffiicalshif…