利用荧光响应的台式生化需氧量传感仪器的研制

利用氧荧光猝灭原理研制了台式生化需氧量(BOD)传感检测仪器。仪器的工作系统由检测系统和软件系统两部分组成。该检测仪操作简便,检测快速,可进行海水BOD含量的现场检测。仪器的性能考察结果表明,在0.5~50mg/L浓度范围内BOD响应的线性相关系数为0.9978。实际海水样品的检测结果显示,仪器对海水样品的平行测定结果相对标准偏差小于±5%,并且与标准五日生化需氧量(BOD5)方法所获得的数值的相关性为0.99。仪器具有较长的使用寿命和良好的稳定性。     

英国牛津仪器超导部宣布调整产品战略

2006年2月16日英国牛津仪器超导部宣布调整产品战略：未来将着重于高科技含量的高端NMR磁体、DNP-NMR磁体系统的研发，并向各大学、科研院所及生产研发部门等研究领域直接供应核磁共振磁体。这样的策略调整对于该领域的客户来说，无疑是一条利好消息，因为如此的销售模式可以使客户省却中间环节直接从磁体的生产厂家购买到磁体，从而得到最低的价格和更多的磁体、谱仪选择空间，以及获得来自磁体生产厂家更专业、周到的售后服务。     

化学发光消耗型锰传感器

化学和生物发光是由化学反应产生的一种光辐射,不需要任何光源。又由于它们具有高灵敏度、宽线性范围和相对比较便宜的仪器等优点,因而在化学和生物传感器领域引起了广泛的兴趣。已用于H_2O_2、乳酸和胆固醇等多种生物活性物质的测定,但未见有金属离子传感器的报道。本文发展了一种新型的全固态模式的消耗型锰离子化学发光传感器。该传感器将除待测物外的所有化学发光反应试剂全部固定在阴离子交换树脂Amberlyst A-27上,于化学发光反应之前,将一定量化学发光试剂从固定化试剂柱上洗脱,与样品中的锰离子产生化学发光。已成功地应用于水样中痕量锰离子的测定。每个固定化试剂柱可连续使用100次以上。 1 实验部分 1.1 仪器和试剂 化学发光传感器由流动系统和检测系统两部分组成。其中流动系统主要由蠕动泵、六通阀、固定化试剂柱和流通池组成。检测系统由光电信增管、负高压、放大器和记录仪组成(图1)。     

便携式病害猪肉速测仪的研制与应用

基于健康与病害猪肉中过氧化物酶(POD)的活性不同的原理,研制出便携式的病害猪肉速测仪,用于病害猪肉的检验与鉴别,以评判猪肉的品质。仪器的工作系统由检测系统和软件系统两部分组成。该检测仪具有操作简便,检测快速,可进行现场检测等优点。在对市场猪肉的检测中,利用测定体系与POD的反应动力学曲线,可快速准确地完成病害猪肉的鉴别,健康猪肉和病害猪肉的符合率分别为100%和96%。     

测量复方药物溶出度的全自动药物溶出度测定仪

自行设计组装了一套可以同时测定复方药剂的全自动药物溶出度测定仪.该仪器由光学检测系统(由光源、流动型吸收池,小型光谱仪组成)、自动进样系统、控制与数据处理系统和机械搅拌系统4部分组成.光学系统的检测器是线阵电荷耦合器件(CCD),故可进行同时全光谱采集.数据处理部分采用了自行设计的基于径向基函数的人工神经网络进行浓度预测.用本装置对市售复方药剂鲁南贝特进行的溶出度测量表明,测量的精密度高,准确度较高,分析速度快,样品无需前处理.     

倏逝波全光纤免疫传感器的开发及性能研究

利用倏逝波与荧光免疫分析原理,研制了一种倏逝波全光纤免疫传感器。该系统利用单多模光纤耦合器,使得激发光的传输、荧光的收集与传输均通过光纤来实现,减少了系统的光学分离元件,结构简单、紧凑、可实现仪器小型化;同时该系统光传递效率高、损耗低、信噪比高;单多模光纤耦合器和探头之间采用可拆卸的连接结构,可以实现多种样品的顺序检测。研究表明:光纤探头的最佳锥角度为0.37;系统对Cy5.5荧光染料的检测灵敏度可达到10-9mol/L;系统检测Cy5.5标记的羊抗大鼠IgG的最低浓度为10μg/L,检测时间为10min。     

稀土—铁—氮化合物Sm2（FeM）17Ny永磁材料的稳定性

最近,Coey J.M.D.和Sun Hong等发现了一种具有优异内禀磁特性的化合物Sm_2Fe_(17)Ny,其H_A=14 T Tc=475℃,μ_oM_s=1.54 T。用机械合金化法制得了内禀矫顽力_iH_c=23.5 kA/cm(30kOe)的各向同性磁体,该磁体具有较好的温度特性,例如,在200℃时,其_iH_c=8.8 kA/cm(11.0kOe)。该化合物有一个致命的弱点,就是在650℃附近完全分解为SmN和α-Fe的混合物。因而限制了用烧结法和热形变法制备各向异性磁体     

测量复方药物溶出度的全自动药物溶出度测定仪

自行设计组装了一套可以同时测定复方药剂的全自动药物溶出度测定仪。该仪器由光学检测系统（由光源、流动型吸收池，小型光谱仪组成）、自动进样系统、控制与数据处理系统和机械搅拌系统4部分组成。光学系统的检测器是线阵电荷耦合器件（CCD），故可进行同时全光谱采集。数据处理部分采用了自行设计的基于径向基函数的人工神经网络进行浓度预测。用本装置对市售复方药剂鲁南贝特进行的溶出度测量表明，测量的精密度高，准确度较高，分析速度快，样品无需前处理。     

双编码阿达玛变换光谱法：原理,仪器及光谱分析研究

本文根据阿达玛变换的原理研制成一种双编码阿达玛变换光谱仪，与单编码及常规光谱仪相比，该仪器具有高信噪比、高输入和单检测器多通道同时检测的优点。试样分析表明：该仪器能用于荧光谱分析和原子线光谱分析。     

ZrB2对烧结Sm(Co0.717Fe0.15Cu0.10Zr0.033)7.2合金微观组织和性能的影响

通过在制粉阶段添加微量ZrB2粉末的方法,制备了Sm（Co0.717Cu0.1Fe0.15Zr0.033）7.2（ZrB2）x（x=0～0.025）烧结磁体.采用扫描电子显微镜、能谱分析和X射线衍射分析磁体的微观组织及相组成,利用NIM-2000型直流磁性测量仪测试磁体的磁性能,研究了添加ZrB2对永磁体组织性能的影响.结果表明： 适量添加ZrB2可以降低磁体的烧结温度; ZrB2发生部分分解会影响合金组织与结构,使合金室温磁性能和高温稳定性都有不同程度的提高; 没有分解的ZrB2颗粒以质点的形式存在,使磁体的断裂韧性值大幅度增加.     

Analysis of a coloured Dutch map from the eighteenth century: the need for a multi-analytical spectroscopic approach using portable instrumentation

A Dutch map from the eighteenth century was multi-analytically analysed making use of energy dispersive X-ray fluorescence (EDXRF), Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), Raman and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS). The cellulosic support was characterised and its state of conservation was evaluated. Besides, paramagnetic impurities were detected together with copper metallic chips. The colours present in some areas of the map were also analysed. Vermilion, carbon black and organic pigments were found. Surprisingly, in the green areas, the rare presence of the mineral moolooite (copper oxalate) was detected. A possible biological attack is discussed in order to explain the presence of such compound. Almost all of the techniques used in the analysis were portable, non-destructive and non-invasive, which is very desirable when analysing objects belonging to Cultural Heritage. The need for a multi-analytical approach using portable instrumentation is also discussed.     

低场核磁共振法对油基钻井液乳状液乳滴稳定性的研究

采用低场核磁共振技术,针对油基钻井液油包水型乳状液乳滴的稳定性进行研究。引入弛豫试剂Mn Cl2·4H2O对W/Q型乳状液的T2分布曲线进行定性分析,位于10~1 000 ms之间的弛豫峰对应于中度可自由移动水和白油弛豫峰的叠合峰,定义为乳状液弛豫峰;1 000~10 000 ms之间的峰为高度可自由移动水的弛豫峰。基于此,以弛豫峰峰形为定性指标,弛豫峰面积比率和弛豫峰间距为定量指标,针对弛豫试剂、油水比和老化温度等因素对乳状液横向弛豫时间T2分布曲线的影响进行了分析,进而深入研究了其对油基钻井液乳状液乳滴稳定性的影响。还将低场核磁共振分析技术运用于油基钻井液乳状液体系相对含油率的测量。结果表明,低场核磁共振是一种高效、快捷、准确反映油基钻井液乳状液稳定性的分析测试技术,同时,还可用于油基钻井液乳状液或原油相对含油率的测量。     

Solid-state 31P NMR spectroscopy of precipitated guanine nucleotide-binding protein Ras in complexes with its effector molecules Raf kinase and RalGDS

Liquid-state 31P NMR spectroscopy is a well-established method for the study of guanine nucleotide-binding proteins (GNB proteins) such as the proto-oncogene Ras. Solid-state 31P NMR spectroscopy could meanwhile also be used to study microcrystalline samples of Ras as well as its partial loss-of-function mutants Ras(T35S) and Ras(T35A). However, solid-state NMR studies of the latter mutants in complex with effector molecules such as RalGDS or Raf kinase were so far prevented, since it has been impossible to crystallize these complexes yet. The aim of the present contribution is to make such complexes accessible to solid-state 31P NMR spectroscopy by the application of precipitation methods. The complex formed by Ras(T35S) and Raf kinase is preserved during precipitation. In contrast, the weakly bound complex of Ras(T35S) with RalGDS is dissociated or at least perturbed by the precipitation procedure. Solid-state 31P NMR experiments on precipitates of these complexes deliver spectra of high resolution and signal-to-noise ratio which allows the application of two-dimensional techniques. Precipitates prepared using polyethylene glycol 6000 (PEG) as precipitant were found to exhibit spectra of maximum resolution and signal-to-noise ratio. Interestingly, the 31P signal due to the alpha-phosphate of GppNHp bound to Ras(T35S) in crystalline samples or aged precipitates has a significantly different isotropic chemical shift than in the liquid state or in freshly prepared precipitates. This directly indicates that the crystal structure differs from the equilibrium solution structure at least in the neighborhood of the alpha-phosphate group.     

停流技术在生物化学分析中的应用

本文全面评述了停流技术的研究现状及发展,讨论了典型的仪器装置及其在生化分析中的应用。     

Measurements of fluoride in bone biopsies by neutron activation analysis for the clinical study of osteoporosis

A procedure has been developed to measure fluoride concentration in bone biopsies by neutron activation analysis /NAA/. The NAA procedure is non-destructive so that the bone biopsies can be used subsequently for histological evaluation. The fluoride content is expressed as F/Ca ratio in the bone samples. The fluoride and calcium are measured using the reactions:¹⁹F/n, /²⁰F /t=11.2 s/ and⁴⁸Ca/n,/⁴⁹Ca/t=8.8 m/, respectively. The F/Ca ratio normalizes the fluoride to bone mineral avoiding the use of bone weight which is unreliable with fresh biopsy samples. This ratio also corrects for variations in neutron flux and gamma counting efficiencies. Results by this procedure were compared to biochemical determinations using an ion-selective electrode for fluoride and atomic absorption for calcium. The two methods gave results which agreed within ±5% which is the precision of the NNA procedure. The NAA method provides a simple and non-destructive procedure for fluoride measurement in bone biopsies for clinical studies. The method is now routinely used in our clinical studies for the fluoride measurements on biopsies from osteoporotic patients treated with fluoride therapy for nearly four years.     

Critical investigation of coupled liquid chromatography–NMR spectroscopy in pharmaceutical impurity identification

In this paper, we investigate the application of coupled LC–NMR to the identification of low‐level impurities. We consider the absolute sensitivity of the technique with our instrumentation, and how this is degraded by peak broadening on and after column, and we compare the sensitivity and other aspects of LC–NMR with a more classical approach of impurity isolation and tube NMR. We show that despite the undoubted advantages of LC–NMR in many situations, for the identification of very low‐level impurities it may not always be the most efficient overall approach when all factors are considered. Copyright © 2003 John Wiley & Sons, Ltd.     

聚乙二醇-聚二氧六环酮嵌段共聚物的合成及表征

用辛酸亚锡［Ｓｎ（Ｏｃｔ）２］作催化剂，进行了端羟基聚乙二醇（ＰＥＧ）和１，４ 二氧六环酮（ＤＯＮ）的共聚反应，得到嵌段共聚物ＰＤＯＮ ｂ ＰＥＧ ｂ ＰＤＯＮ．根据１Ｈ ＮＭＲ谱图计算结果表明共聚物组成随两组分投料比而改变．共聚物的ＤＳＣ结果表明嵌段共聚物中ＰＤＯＮ的熔点和结晶度的变化相对较小，而ＰＥＧ的熔点及结晶度均有较大降低．将ＰＥＧ引入可大大提高材料的吸水率．     

一种改进方法合成六（4－硝基酚氧）环三磷腈

报道合成六（4-硝基酚氧）环三磷腈的一种改进方法,该法大大缩短了反应时 间（约1.5 h）,简化了操作。产物经红外、核磁氢谱和磷谱的分析、元素分析以 及差示扫描量热分析。     

氧化硼对苯乙烯原子转移自由基聚合的加速作用

以2-溴丙酸乙酯为引发剂, 溴化亚铜为催化剂, N,N,N′,N″,N″-五甲基二乙基三胺为配体, 以氧化硼为加速剂, 进行了苯乙烯原子转移自由基聚合的加速研究. 发现氧化硼与引发剂比例为4时, 加速效果最为明显, 且对分子量的控制效果较好. 在85 ℃时, 添加该比例的氧化硼, 苯乙烯在6 h的聚合转化率达到78.5%. 在65, 75及85 ℃条件下, 加入氧化硼时体系的聚合反应动力学为一级反应, 苯乙烯聚合速率分别为空白体系的1.82, 1.54和1.5倍; 聚合物的分子量可控, 分子量分布窄, 体系呈现明显的活性聚合特征. 通过核磁共振谱对聚合物的结构进行了表征, 证明氧化硼在整个聚合过程中只起加速作用, 并不影响聚合机理和聚苯乙烯的结构. 氧化硼价廉, 有利于实现原子转移聚合的工业化.     

Rapid identification of common hexapyranose monosaccharide units by a simple TOCSY matching approach

Solution NMR spectroscopy is a well established technique for non-destructive characterization of the structures and conformations of complex oligo- and polysaccharides. One of the key experiments involves the use of 2D TOCSY to collect the 1H spins into groups that can be associated with the individual saccharide units that are present in the molecule under study. It is well known that the magnetization transfer rate through the 1H spin system during the TOCSY spin lock period is sensitive to the intervening 3J(H,H) scalar couplings, and therefore also to the saccharide stereochemistry. Here, we have investigated the potential to extract information on the stereochemistry of hexapyranose monosaccharide units directly from TOCSY spectra. Through a systematic experimental investigation of the magnetization transfer initiated from the anomeric 1H resonance in D-glucose, D-galactose and D-mannose it is shown that a 100 ms spin lock time provides optimal spectroscopic discrimination between these three commonly occurring building blocks. A simple matching scheme is proposed as a new tool for rapid attribution of the TOCSY traces originating from the anomeric 1H resonances towards the underlying monosaccharide type. The scheme appears robust with regard to structural variations and fairly tolerant to incidental overlap. Its application provides useful guidance during the subsequent NMR assignment process, as demonstrated with the PS7F polysaccharide from Streptococcus pneumonia. In addition, we show that our scheme affords a clear-cut distinction between the alpha- and beta-epimers of D-mannose-type units, which can be difficult to discriminate by NMR analysis. Application to the N-glycan 100.2 demonstrates the potential and wide applicability of this new discrimination approach.