19F-NMR外标法测定盐酸左氧氟沙星中的氟含量

本文研究了利用19F-NMR技术测定盐酸左氧氟沙星药物样品中氟的检测条件.优化了实验参数,选用三氟乙酸钠作内标,重水与去离子水混合液为溶剂.测定了对盐酸左氧氟沙星样品中氟含量.实验表明,氟的加标回收率在98.4%-100.6%之间,标准偏差为0.00214%-0.0489%,相对标准偏差小于1.124%.     

19F-NMR测定生产钽、铌矿的废液中总氟含量

建立了一种核磁共振波谱测定钽、铌生产的废液中氟含量的方法。研究了氟谱测定的前处理和共存离子的干扰 ,以外标法和内标法进行定量分析。实验结果表明 ,内标法的相对标准偏差为 2 .71% ,回收率在 98.4 %— 10 2 .1%之间 ,外标法的相对标准偏差为 3.31% ,回收率在 97.4 %— 10 3.2 %之间。该法简便、快捷 ,分析结果令人满意     

19F-NMR测定甲磺酸帕珠沙星样品中的氟

研究了19F-NMR技术测定甲磺酸帕珠沙星药物样品中氟的检测条件.优化了实验参数,选用三氟乙酸钠作为内标,重水与去离子水混合液作为溶剂的内标绝对法进行定量分析.测定了甲磺酸帕珠沙星药物样品中氟含量.实验表明,氟的加标回收率在99.2%-100.9%之间,标准偏差为0.00446%-0.0652%,相对标准偏差小于1.459%.     

19F NMR的特点

¹⁹F的磁旋比和相对灵敏度接近质子;¹⁹F NMR化学位移范围可达 δ 1 000,谱图分辨率高;¹⁹F NMR对环境因素较氢谱远为敏感、复杂,可反映出化合物结构的细微差别. 由于正常生物体内含氟成分很少,干扰小,因此在生物医学研究中引入氟代物进行¹⁹F NMR研究有特殊意义. 对氟化物的¹⁹F NMR化学位移和偶合常数的范围也分类作了总结.     

19F NMR化学位移经验公式的影响因素

化学位移是核磁共振技术的重要参数,目前对¹H NMR、¹³C NMR已提出一系列估算化学位移的经验公式,但¹⁹F NMR化学位移规律研究报道则较少,以δ=B+∑△i+C化学位移通式为基础,分析屏蔽常数对化学位移的作用,并针对¹⁹F原子,分析了氟的电子云密度、立体效应、溶剂效应、氢键、标准、浓度和温度等影响因素,对¹⁹F NMR化学位移经验公式的提出提供理论依据。     

19F固体核磁共振技术研究膜蛋白相互作用的进展

固体核磁共振技术因其可实现细胞膜环境中的蛋白质结构研究而广受关注.¹⁹F元素由于灵敏度高、天然丰度高,无生物背景等优点,被广泛应用于生物核磁共振技术中.氟标固体核磁共振技术常被用于细胞膜中蛋白质的相互作用研究,如：抗菌肽与细胞膜的相互作用、聚合膜蛋白结构分析等.此篇综述介绍了常用的蛋白质氟标修饰的实验方法,总结了常用的¹⁹F生物固体核磁共振实验技术,以及介绍了应用¹⁹F固体核磁共振研究膜蛋白的成功案例.此外,此篇综述讨论了¹⁹F固体核磁共振技术在蛋白质研究中的局限性.     

氟苯类化合物19F NMR化学位移的计算

提出了计算氟苯类化合物¹⁹F NMR化学位移的公式：δ_cal（¹⁹F）=-113.5+Δo+Δm+Δp+C, 结合最小二乘法通过线性回归得到了20种取代基参数, 计算结果以160种氟苯类化合物的263个¹⁹F NMR化学位移数据为样本点作回归检验,置信度为99.5%,计算值与实验值的平均偏差为0.628,计算值与实验值的标准偏差为4.720,约有93.2%的¹⁹F NMR化学位移计算值的计算误差<7.0（相对误差<0.7%）.     

19F磁共振波谱分析CD基因在人结肠癌细胞的表达

为了研究¹⁹F-NMR波谱分析胞嘧啶脱氨酶（CD）基因在人结肠癌细胞中表达的可行性,通过逆转录病毒介导方法,将编码大肠杆菌的CD基因转染到人结肠癌细胞系SW1116. 通过RT-PCR、MTT方法和¹⁹F-NMR波谱分析了CD基因在人结肠癌细胞中的表达状况. 结果显示转基因的肿瘤细胞SWCD₂中表达CD基因,对前药5-氟胞嘧啶（5-FC）的敏感性较亲本肿瘤细胞SW1116明显增高,50%细胞生长抑制率（IC₅₀）为66 μmol/L, 而SW1116 细胞IC₅₀为16 mmol/L. ¹⁹F-NMR波谱分析显示,转导CD基因细胞在774 μmol/L 5-FC浓度培养24 h后的样品,在δ -91.7和δ -93.3显示了2个双峰,分别是5-FC和5-氟尿嘧啶(5-FU)的¹⁹F-NMR的信号,提示5-FU是SWCD₂细胞内的CD酶催化5-FC的代谢产物. 这些结果表明¹⁹F-NMR分析是一种能够用于检测CD基因在人结肠癌细胞中表达的新方法,它将有助于对临床基因治疗方案实施监测.      

燃烧法合成SrAl12O19:Eu2+

利用相应的金属硝酸盐和尿素之间发生的氧化还原反应，在600℃的炉温下，制备了发蓝光的铝酸盐发光粉SrAl12O19:Eu^2 ，产物为六方晶系。研究结果表明，在制备Eu^2 激活的铝酸盐发光粉时，适当量的尿素用量和相对密闭的反应体系有利于获得纯相和单一发光颜色的产物。     

聚合物锂离子电池制备技术

目前新一代锂离子电池体系的聚合物锂离子电池不仅具有液态锂离子电池的所有技术优点，而且具有更高的比能量和更好的安全性。更适合应于用。在电极膜的制备方面，需要对活性材料、骨架基质材料、增塑剂、导电剂等正、负极各组分的配比进行优化。采用合适分子量的PVDF—HFP（聚偏氟乙烯-六氟丙烯）为骨架基质材料，DBP（邻笨二甲酸二丁酯）为增塑剂、炭黑为导电剂，能够较好地满足聚合物锂离子电池电极膜及电解质膜的技术要求。     

31P和19F NMR在细胞内游离镁离子测定中的研究

目前有多种分析方法可以测定生物细胞内镁离子的浓度,但这些方法都有一定的弊端,需要将细胞破坏,而且不能进行连续的测定. 核磁共振（NMR）方法是一种可以对活细胞、组织等进行无损伤的测定的技术,允许在较长时间内连续进行观察,可以同时考察胞内、胞外离子浓度. 核磁共振测定生物细胞内镁离子的³¹P NMR 和¹⁹F NMR方法近年来多应用于临床医学、生物分析等方面.      

测定高纯水中痕量杂质Mn、Cd和Cr的原子吸收光谱分析技术

为了克服在环境无净化条件下的污染和采用化学处理预富集而引入较高的空白值，采用了“空气参比－炉内富集－先测样品后测标准”的无火焰原子吸收光谱分析技术，测定高纯水中ｐｐｂ级的痕量元素Ｍｎ、Ｃｄ、Ｃｒ。方法简便，快速。测定各元素的相对标准偏差＜１０％。     

Study of 19Na at SPIRAL

The excitation function for the elastic-scattering reaction p( ¹⁸Ne, p) ¹⁸Ne was measured with the first radioactive beam from the SPIRAL facility at the GANIL laboratory and with a solid cryogenic hydrogen target. Several broad resonances have been observed, corresponding to new excited states in the unbound nucleus ¹⁹Na. In addition, two-proton emission events have been identified and are discussed.     

Precision mass measurements of 40Ca17+ and 40Ca19+ ions in a Penning trap

High-precision mass measurements on lithium-like and hydrogen-like ⁴⁰Ca-ions are reported. The obtained mass of the hydrogen-like and lithium-like ion is 39.952181819(29) u and 39.953272223(24) u, respectively. The corresponding mass of the ⁴⁰Ca atom is 39.962590858(22) u. This new value has a precision ten times higher than the literature value.     

Development of the Argonne positron source APosS

In this paper we discuss the progress at Argonne National Laboratory with the APosS. We outline possible improvements that can increase the flux of positrons by increasing the electron current on target or by modification of the positron converter. We discuss some new techniques that could increase moderation efficiency and thus further increase positron flux two to three orders of magnitude by making use of modern accelerator techniques.     

Polarizing Microscopic and 31P NMR Studies of Decylammonium Chloride/Potassium Chloride/Water System. Containing Phosphoric Acid Monodecyl Ester and H3PO4

The decylammonium chloride (DACl), KCl and D₂O system forms two phases(N_c+N_d) in the nematic range. The N_d phase was ca. 15% by volume and exhibited extinct appearance. From conoscopic measurements it was inferred that the optical axis of the N_d phase was tilted. The lamellar phase of the DACl-KCl-D₂O system as well as the lamellar phase obtained by adding phosphoric acid decylester/phosphoric acid (PDE/H₃PO₄) showed the following phase sequence: L_α + N_d 35°C H_α + N_d 40°C N_c + N_d 45°C N_c 50°C isotropic The line shapes of ³¹P NMR of PDE/H₃PO₄ were found to be sensitive to micelle size and dynamics occuring in the lyotropic system, but they do not differentiate between different micelle shapes.     

Development of an optical trap for microparticle clouds in dilute gases

Long-duration experiments with clouds of microparticles are planned for the ICAPS facility on board the International Space Station ISS. The scientific objectives of such experiments are widespread and are ranging from the simulation of aerosol behaviour in Earths atmosphere to the formation of planets in the early solar system. It is, however, even under microgravity conditions, impossible to sustain a cloud of free-floating, microscopic particles for an extended period of time, due to thermal diffusion and due to unavoidable external accelerations. Therefore, a trap for dust clouds is required which prevents the diffusion of the particles, which provides a source of relative velocities between the dust grains and which can also concentrate the dust to higher number densities that are otherwise not achievable. We are planning to use the photophoretic effect for such a particle trap. First short-duration microgravity experiments on the photophoretic motion of microscopic particles show that such an optical particle-cloud trap is feasible. First tests of a two-dimensional trap were performed in the Bremen drop tower.     

Improved synthesis of polyfluorinated l-lysine for 19F NMR-based screening

Polyfluorinated N-α-Fmoc--Boc-l-lysine represents the best-in-class among a set of polyfluorinated amino acids (PFAs) which are useful tools for ¹⁹F NMR-Based Screening. In this communication, optimized reaction conditions that allowed for the multi-gram preparation of this unnatural amino acid are reported.