GC-FPD、GC-MS法分析血液样品中的毒鼠强

采用液-液提取方法及GC—FPD定量、GC—MS定性检测手段，对血液样品中毒鼠强的提取和检测方法进行了研究。时提取毒鼠强的溶剂类型、溶剂用量及质谱分析参数等因素进行了考察，建立了一种回收率高、重现性好、灵敏度佳、干扰少的毒鼠强分析方法。毒鼠强工作曲线的线性范围为0．01-0．2μg／μL，相关系数r=0．9999，空白血液的加标平均回收率为93．6％，测定结果的相对标准偏差为5．27％。该方法满足司法鉴定中生物样品的定性、定量检验要求。     

简易法制备高量子产率荧光材料及其应用

选用柠檬酸和三乙烯四胺作为原料,在相对低温下(80 ℃),制备量子产率高达78%的荧光材料。 通过紫外吸收、荧光、傅里叶变换红外光谱仪(FTIR)、核磁共振波谱仪(NMR)等技术手段对该体系进行表征。 结果表明,该荧光材料属于非典型性荧光材料,其强荧光性可能源于体系中大量羰基的聚集。 这种高量子产率材料满足制备隐形墨水的要求,在图案化、防伪和光电子设备等领域具有潜在的应用前景。     

气相色谱-质谱法测定生物检材中毒鼠强的含量

采用气相色谱-质谱提取离子的方法测定了生物检材中毒鼠强的含量。毒鼠强的线性范围为0.05-50ng，检出限为0.01ng，以苯为溶剂，毒鼠强的提取回收率为93.5%，RSD为4.96%(n=5)。方法准确、快速，适用于生物检材中毒鼠强的测定。     

Analysis of questioned documents: A review

During the last years (2000–2014), many publications concerning the forensic analysis of questioned documents have been published, and new techniques and methodologies are nowadays employed to overcome forensic caseworks. This article reviews a comprehensive collection of the works focused on this issue, including dating studies, the analysis of inks from pens and printers, the analysis of paper, the analysis of other samples related to questioned documents and studies on intersecting lines. These sections highlight the most relevant analytical studies by a wide range of analytical techniques. Separation and spectrometric techniques are critically discussed and compared, emphasizing the advantages and disadvantages of each one. Finally, concluding remarks on the research published are included.     

Styryl-Telechelic Polyisobutylenes. I. Synthesis of Linear and Tri-Arm Star Styryl-Telechelic Polyisobutylenes

New linear and three-arm star polyisobutylenes carrying two and three terminal styryl endgroups, i.e., F_n = 2.0 and 3.0, respectively, have been prepared. The synthesis of these styryl-telechelic polyisobutylenes involved Friedel-Crafts alkylation by linear and/or three-arm star polyisobutylenes carrying tertiary chlorine endgroups of (2-bromoethyl)benzene or /β-bromoisopropylbenzene followed by de-hydrobromination. According to model studies, ¹H-NMR, and UV spectroscopy, the conversions are essentially quantitative. These new terminally di- and tri-styrenated polyisobutylenes may be useful for the preparation of block copolymers and as cross-linking materials.     

一锅法合成二硝基五亚甲基四胺反应机理的研究

二硝基五亚甲基四胺(DPT)是高性能单质炸药奥克托金(HMX)的重要硝化前体.以尿素为起始原料,中间产物不分离,经硝化、水解、Mannich缩合等反应得到DPT,总收率63.2%.通过分离、捕获中间体以及同位素示踪实验研究了一锅法合成DPT的反应机理.分离出了稳定的中间体二硝基脲、硝酰胺和二羟甲基硝酰胺,用苯磺酰氯捕获到了活性中间体1-硝基-六氢均三嗪.以氘代甲醛、二羟甲基硝酰胺和氨缩合得到氘标记的DPT,1HNMR和MS分析结果表明:在反应过程中二羟甲基硝酰胺解离释放出甲醛和硝酰胺,小分子碎片随机组合生成了三嗪化合物,进而生成DPT.     

Mono- or narrow disperse poly(methacrylate-co-divinylbenzene) microspheres by precipitation polymerization

Precipitation copolymerizations of five mono-vinyl methacrylic monomers including methyl methacrylate (MMA), butyl methacrylate (BMA), dodecyl methacrylate (DMA), glycidyl methacrylate (GMA), and hydroxyethyl methacrylate (HEMA) with divinylbenzene (DVB), in a wide range of comonomer composition, were carried out in acetonitrile to form mono- or narrow disperse crosslinked copolymer microspheres. In addition, two divinyl methacrylic monomers, ethylene glycol dimethacrylate (EGDMA) and triethylene glycol dimethacrylate (TEGDMA), were also copolymerized with DVB, and optionally a third comonomer (GMA or HEMA), to yield similar microspheres in acetonitrile. The possibility of creating porosity was explored for some of the copolymer particles. All these microspheres have clean surfaces due to the absence of any added steric or ionic stabilizer, and they are in the size of the micrometer range, varying from 1 to 7 µm, depending on the type and content of the methacrylic comonomer. Particle size distribution, surface morphology, internal texture, and porosity properties of these particles were studied by a Coulter Multisizer, a scanning electron microscope, a transmission electron microscope, and an Autosorb-1. The effects of comonomers on microsphere formation and morphology are described. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 2899–2907, 1999     

生物检材中毒鼠强的GC-MS选择离子分析

采用二氢甲烷萃取GC－MS及选择离子定性的方法,检测了血液、尸体脏器中的灭鼠药毒鼠强（四次甲基二砜四胺）,毒氧强分子量为240,其质谱图中有明显的分子离子峰240m/z、基峰42m/z及212、185、132、121、92、76m/z的碎片离子峰。对212、240m/z碎片离子进行扫描,可提高检测灵敏度。本法适用于中毒血液和脏器中低含量毒鼠强的定性检测。     

合成8-氨基-3,6-二氧杂辛酸前体的新方法

合成8-氨基-3;6-二氧杂辛酸前体的新方法;二缩三乙二醇;二缩三乙二醇单对甲苯磺酸酯;邻苯二甲酰亚胺基二氧杂辛醇;氨基二氧杂辛酸;合成     

气相色谱-质谱联用法同时测定烟草中的1-丙醇、二甘醇、三甘醇、丙二醇与丙三醇

将烟草样品粉碎至40目,以1,4-丁二醇为内标,甲醇为萃取溶剂,超声萃取60 min后,以气相色谱-质谱/选择离子监测(GC-MS/SIM)法测定1-丙醇、二甘醇、三甘醇、丙二醇和丙三醇的含量。结果表明:目标化合物在1~100μg/mL范围内线性关系良好,方法的检出限为0.05~0.48μg/mL,回收率为90.2%~103.7%,相对标准偏差(RSDs)为0.9%~3.0%。方法的前处理简单、灵敏度高、定性定量准确,适用于烟草中多元醇的定性定量分析。