毛细管电泳发光二极管诱导荧光对免疫球蛋白G的检测

采用自行设计、组装的毛细管电泳光导纤维发光二极管诱导荧光检测装置,建立了一种直接测定免疫球蛋白G(IgG)的方法。以蓝色发光二极管(LED)为荧光检测器的激发光源,荧光素异硫氰酸酯(FITC)为柱前衍生试剂,采用毛细管区带电泳,以20 mmol/L硼砂缓冲溶液(pH9.2)为背景电解液进行分离检测。通过对衍生反应条件和电泳分离条件进行优化,确定了最佳实验条件,在该条件下,IgG的线性范围为4.5×10-8~1.2×10-6g/L,检出限为2.0×10-8g/L。该方法简单、高效、选择性好,无需前处理,可用于人血清中IgG含量的测定。     

尿样中神经性毒剂代谢产物的HPLC/Q-TOFMS/MS检测方法研究

建立了尿样中甲基膦酸单乙酯(EMPA)、甲基膦酸单异丙酯(IMPA)、甲基膦酸频哪基酯(PMPA)3种神经性毒剂代谢产物的HPLC/Q-TOFMS/MS检测方法。以StrataSi-1型固相萃取小柱对尿样中的3种神经性毒剂代谢产物进行分离,HPLC/Q-TOFESIMS/MS进行测定,内标法定量。该方法对EMPA、IMPA、PMPA的线性范围均为5～320μg/L,相关系数均不低于0.9974;EMPA、IMPA、PMPA的加标回收率分别为57%、98%、81%;检出限(S/N≥3)均为0.1μg/L,定量下限(S/N≥10)均为1μg/L。并将该方法应用于禁化武组织(OPCW)首次生物医学样品分析演练未知尿样的检测,结果满意。     

克百威分子印迹聚合物的合成及其性能评价

以克百威为模板分子,甲基丙烯酸(MAA)为功能单体,二甲基丙烯酸乙二醇酯(EGDMA)为交联剂,采用沉淀聚合的方法制备了克百威分子印迹聚合物。通过红外光谱分析得到模板和功能单体的最佳配比为n(carbofuran)∶n(MAA)=1∶6。印迹聚合物的红外光谱测定结果表明,聚合物中存在与模板分子相互作用的特征基团;从印迹聚合物的扫描电镜图观察到分子印迹聚合物(MIP)与空白聚合物(NIP)的表面形态不同,可推论MIP存在与模板分子相互识别的结合位点。通过静态平衡结合法研究了模板分子聚合物的吸附能力、结合动力学和选择特性。结果表明,与非印迹聚合物相比,印迹聚合物对克百威具有较强的吸附特性和很好的专一选择性,3h后基本达到最大吸附量。采用固相萃取柱预处理样品,用高效液相色谱法测定自来水中10、50、100mg/L克百威的加标回收率为94%～117%,相对标准偏差(n=3)为2.5%～4.7%。     

新药唑来膦酸钠的合成工艺改进

在离子液体{[bmin]BF4}中,以咪唑-1-基乙酸盐酸盐为原料,通过缩合和水解反应合成了新药唑来膦酸钠,总收率60.0%,纯度99.8%,其结构经1HNMR和IR表征。[bmin]BF4可回收套用。     

Differential Expression of Molecular Chaperones in PC12 Cells Treated with PSI

<正>Parkinson's disease(PD) is a common neurodegenerative disorder whose primary pathology features are the degeneration of dopaminergic neurons in the substantia nigra pars compacta(SNc) and the presence of eosinophilic inclusions called Lewy body in the cytoplasm of the remained neurons.Growing evidence suggests that dysfunction of the ubiquitin-proteasome system(UPS) is involved in the etiopathogenesis of PD.In order to investigate the pathogenetic mechanism of ubiquitin-proteasome dysfunction in PD,2D-differential gel electrophoresis (2D-DIGE) and MALDI-TOF Pro MS were used to determine the proteins,which were differentially expressed,in PC12 cells that had undergone a synthetic proteasomal inhibitor PSI(10μmol/L) treatment for 24 h.Forty-six protein spots were differentially expressed in response to PSI administration,of which 34 were increased and 12 decreased. Six of these were identified as molecular charperones:endoplasmin precursor(GRP94),heat shock protein 105(HSP105),HSC-70-psl,glucose ruglated protein 75(GRP75),glucose ruglated protein 58(GRP58) and heat shock 27000 protein 1(HSP27).The results suggest that the molecular chaperones play an important role in the PD model induced by proteasomal inhibitor.     

Evaluation of Thermal Hazard of Composite Modified Double-base Propellant by Microcalorimetery Method

<正>The thermal decomposition behavior of composite modified double-base(CMDB) propellant containing cyclotrimethylene trinitramine(RDX) was studied via a Calvet microcalorimeter at five different heating rates.The activation energy(E) and the pre-exponential factor(A) of two obvious exothermic processes were obtained by Kissinger's method and Ozawa's method.The entropy of activation(△A~≠),the enthalpy of activation(△H~≠),and the free energy of activation(△G~≠) of the first stage were calculated.To evaluate the thermal hazard of the RDX-CMDB propellant, the critical temperature of thermal explosion(T_b),the self acceleration decomposition temperature(T_(SADT)),the adiabatic decomposition temperature increment(△T_(ad)) and the time-to-explosion of adiabatic system(t) were presented as 145.3℃,138.15℃,1634 K and 583.71 s(n=0) and 586.28 s(n=1),respectively.     

Physical and Electrochemical Characterization of Hydrothermal Prepared α'-NaV_2O_5 Crystals

α'-NaV2O5 was prepared by a simple hydrothermal process.X-ray diffraction confirmed the orthorhombic structure of α'-NaV2O5,with preferential growth along the (001) direction.Scanning electron microscopy showed α'-NaV2O5 was composed of flake-shaped crystals.X-ray photoelectron spectroscopy confirmed the co-existence of V4+ and V5+ in α'-NaV2O5,which results in an average V4.5+ oxidation state of α'-NaV2O5.The observed Raman bands are ascribed to different V―O vibrations.α'-NaV2O5 shows a reversible specific capacity of about 100 mA·h·g-1 between 3.5 and 1.0 V,with a good capacity retention.The good electrochemical stability of the material is attributed to its structural stability during Li+ intercalation.     

Estimation of Critical Temperature of Thermal Explosion for Trinitromethyl Explosives by Non-isothermal DSC

Two general expressions and their six derived formulae for estimating the critical temperature(Tb) of thermal explosion for energetic materials(EMs) were derived from the Semenov’s thermal explosion theory and eight non-isothermal kinetic equations via reasonable hypothesis. We can easily obtain the values of the initial temperature(T0i) at which DSC curve deviates from the baseline of the non-isothermal DSC curve of EMs, the onset temperature(Tei), the exothermic decomposition reaction kinetic parameters and the values of T00 and Te0 from the equation T0i or ei=T00 or e0+α1βi+α2βi2+···+αL–2βiL–2, i=1, 2, ···, L and then calculate the values of Tb by means of the six derived formulae. The results obtained with the six derived calculating methods for six trinitromethyl explosives: bis(2,2,2- trinitroethyl-N-nitro) ethylene diamine(BTNEDA), 2,2,2-trinitroethyl-4,4,4-trinitrobutyrate(TNETB), bis(2,2,2- trinitroethyl) formal(BNTF), bis(2,2,2-trinitroethyl-nitramine)(BTNNA), 2,2,2-trinitroethyl-2,2,2-trinitroethyl-N- nitroamino acetate(TNTNNA) and tetrakis [2,2,2-trinitroethyl] orthoester(TTNOE) agree well with each other.     

预烧温度对CaO-Li_2O-Sm_2O_3-TiO_2微波介质陶瓷介电性能的影响

用固相反应法制备了CaO-Li2O-Sm2O3-TiO2(CLST)微波介质陶瓷。通过改变预烧温度(1 000~1 200℃)研究其对CLST微波介质陶瓷介电性能的影响。研究过程中,对预烧粉体与烧结陶瓷进行XRD与SEM分析,对陶瓷的介电性能εr、Q、τf进行了测试。结果表明,预烧温度对CLST微波介质陶瓷介电性能有较大影响,在预烧温度1 150℃,烧结温度1 340℃时可获得较好的介电性能:εr=112,Q=845,τf=52×10-6/℃。     

气相色谱-表面声波快速分析仪性能评价

本文评价了自行研制的气相色谱-表面声波(GC-SAW)联用快速分析仪的性能。实验结果表明:在6 s以内,GC-SAW快速分析仪能分离五种苯系物和C6~C14九种正构烷烃。该仪器对甲苯测定的相对标准偏差(RSD)为2.5%(n=6);最小检出浓度为2.05μg.L-3;线性范围为2.05~205μg.L-3;对标准样品连续6次分析,经双边t检验,分析结果均值与标样标准值无显著差异。