手性固定相NP-HPLC拆分达非那新中间体对映体

采用多糖衍生物手性色谱柱,建立了正相高效液相色谱法(NP-HPLC)拆分达非那新中间体对映体.考察了该对映体在不同手性固定相上的分离趋势及保留顺序,以及流动相组成对该中间体对映体的分离度和洗脱顺序的影响.结果表明:用Chiralpak AD和Chiralcel OJ柱均能实现对映体的有效分离,为达非那新中间体的光学纯度...     

手性固定相正相高效液相色谱法拆分普萘洛尔对映体

建立了手性固定相正相高效液相色谱拆分普萘洛尔对映体的方法,考察普萘洛尔对映体在4种多糖类手性色谱柱(Chiralpak AD柱、Chiralcel OD柱、Cniralcel OJ柱和Chiralpak AS柱)(Daicel,250mm×4.6mm,10μm)上的分离行为,同时考察了流动相中醇类以及碱性添加剂二乙胺(...     

敌草胺对映体圆二色光谱表征及其水体中微量对映体含量测定

应用手性Chiralpak OJ-H柱对除草剂敌草胺进行分离,对其两个对映体用圆二色光谱进行了表征。在此基础之上,应用荧光检测器建立了测定水体中微量敌草胺对映体的测定方法。该方法外消旋体线性范围为10～100 ng·mL-1;外消旋体最低检测限为8 ng·mL-1,对映体纯的检测限为4 ng·mL-1。该方法对于测定环境水体中敌草胺的手性选择性累积具有现实意义。     

紫外分光光度法测定配合物组成及其在手性分离中应用

采用紫外分光光度法测定了Cu(Ⅱ)和L-组氨酸二元配合物的组成及Cu(Ⅱ)与L-组氨酸和泮托拉唑三元配合物组成,研究了配合物的紫外吸收光谱性质,考察了溶液pH对配合物稳定性的影响。Cu(Ⅱ)和L-组氨酸二元配合物的组成比为1∶2,Cu(Ⅱ)与L-组氨酸和泮托拉唑三元配合物组成比为1∶1∶1,碱性条件有利于配合物的生成。该结果应用于高效液相色谱法分离泮托拉唑对映体,分离度为1.4。     

两种二苯醚类除草剂在直链淀粉液相色谱手性固定相上的拆分

以硅胶涂敷直链淀粉-三(5-氯-2-甲基苯基氨基甲酸酯)为手性固定相,对两种含有1个手性中心的二苯醚类除草剂2-甲氧基-2-{5-[2-氯-4-(三氟甲基)苯氧基]-2-硝基苯)丙酸甲酯和乳氟禾草灵,进行了色谱分离.考察了流动相中异丙醇和正己烷的体积比对乳氟禾草灵对映体分离的影响.结果显示,这2种二苯醚类除草剂可以同时在Chiralpak AY-H色谱柱上获得较好的手性拆分结果；并对农药对映体与固定相之间的保留机理进行了讨论.     

共振瑞利散射探针罗丹明B手性识别肉碱对映体

手性对映体广泛存在于环境和生命体中,手性识别有助于探索手性世界的奥妙和生命过程的机理。共振瑞利散射因其灵敏度高成为了手性识别的一大工具。不经分离而同时测定手性对映体则是手性识别的一大新的探索。最近,我们发现罗丹明B可以作为一种散射探针来同时测定肉碱对映体。根据偏振实验可以证明罗丹明B与肉碱反应体系的共振辐射光是由共振荧光和散射光组成。当肉碱对映体与罗丹明B反应时,罗丹明B的共振瑞利散射会有不同程度的增加。根据罗丹明B响应两种对映体RRS信号的差异,我们可以同时测定肉碱对映体。     

基于功能化的金纳米的共振瑞利散射方法手性识别肉碱对映体（英文）

一种不经分离而同时测定手性对映体的简便方案是非常有趣和有用的。提出一种基于共振瑞利散射(RRS)光谱技术手性识别新方法,利用功能化的金纳米粒子(Au NPs)同时检测肉碱对映体。AuNPs的RRS强度很弱,但当Cu~(2+)存在时,RRS强度显著增加。更有趣的是,肉碱对映体均可以降低Cu~(2+)-Au NPs体系的RRS强度,但D-肉碱使RRS降低更多。在最优实验条件下,均有良好的线性关系并有很好的相关系数以及较低的检出限。由此,这种方法可以计算出肉碱对映体的对映体比率和对映体分数。并应用于胶囊样品中肉碱对映体混合物手性识别的研究。该方法不需要复杂的手性修饰处理,并具有简捷低消耗、灵敏度高、选择性好等优点。     

基于功能化的金纳米的共振瑞利散射方法手性识别肉碱对映体

一种不经分离而同时测定手性对映体的简便方案是非常有趣和有用的.提出一种基于共振瑞利散射(RRS)光谱技术手性识别新方法,利用功能化的金纳米粒子(Au NPs)同时检测肉碱对映体.Au NPs的RRS强度很弱,但当Cu2+存在时,RRS强度显著增加.更有趣的是,肉碱对映体均可以降低Cu2+-Au NPs体系的RRS强度,但D-肉碱使RRS降低更多.在最优实验条件下,均有良好的线性关系并有很好的相关系数以及较低的检出限.由此,这种方法可以计算出肉碱对映体的对映体比率和对映体分数.并应用于胶囊样品中肉碱对映体混合物手性识别的研究.该方法不需要复杂的手性修饰处理,并具有简捷低消耗、灵敏度高、选择性好等优点.     

纤维素衍生物手性固定相HPLC拆分非洛地平对映体

采用高效液相色谱法(HPLC),在硅胶涂敷纤维素三-(4-甲基苯甲酸酯)手性固定相上拆分非洛地平.研究了异丙醇体积含量、流速及柱温对非洛地平对映体拆分行为的影响.同时还模拟了在制备分离条件时,增大进样体积和进样浓度对非洛地平拆分的影响.并结合色谱理论和热力学理论对非洛地平的手性识别机理进行探讨.实验表明在正己烷∶异丙醇...     

柱前衍生化RP-HPLC拆分盐酸洛美沙星对映异构体

以2,3,4,6-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)为柱前衍生化试剂,建立了盐酸洛美沙星对映体柱前衍生化RP-HPLC拆分方法。采用了C18(4.6×250mm,5μm,Bnentnach)为色谱柱,在流动相为甲醇∶(3mmol.L-1四丁基溴化铵水溶液∶5mmol.L-1Na2HPO4的水溶液=1∶2)=25∶75,流速为1mL·min-1,检测波长284nm的色谱条件下,盐酸洛美沙星的非对映体在1.0—27.5μg.mL-1的浓度范围内有良好的线性关系,日内、日间精密度都3%,且获得了基线分离。该种方法能用于盐酸洛美沙星的手性拆分,也为盐酸洛美沙星的光学异构体的测定提供了参考。     

基于径向基函数网络的激光诱导荧光特征光谱分离算法

应用激光诱导荧光技术测量水中溶解有机物(DOM)含量，具有灵敏度高、检测速度快、可遥测等优点，其中特征荧光光谱的分离在系统中占有十分重要的地位.在分析激光诱导荧光光谱特征的基础上，提出了采用径向基函数网络(RBFN)分析荧光光谱数据的数学模型，应用这种模型从荧光光谱中恢复出了激光、拉曼和DOM的荧光等光谱分量成分，从而得到了水中DOM的浓度. 关键词： 径向基函数网络 激光诱导荧光 溶解有机物     

Properties and Preparation of Chitosan/Silanol Quaternary Ammonium Modified Silica Hybrids Using Sol–Gel Process

Chitosan/modified silica nanocomposites, with a sol–gel process being used to prepare a silanol quaternary ammonium modified silica possessing antimicrobial activity, were investigated, as well as the thermal properties, morphology, optical, mechanical, antimicrobial, and adsorption properties of this type of nanocomposite. Grafting of the modifier onto nanosilica was confirmed through the Fourier transform infrared (FTIR) spectra. X-ray diffraction patterns indicated that the chitosan structure was not disrupted from the incorporation of the modified silica. Fracture surfaces with no clear micro-phase separation were observed by scanning electron microscopy (SEM), which indicated the good interaction of chitosan and the modified silica. The organic modifier tended to cause the aggregation of the modified silica at higher content on a submicron scale based on transmission electron microscopy (TEM) analysis, which might be due to a decrease of the stability factor originating from the negative charges on silica. With the introduction of modified silica, the optical transmittance decreased at higher organic modifier content in agreement with TEM analysis. The elongation at break remained largely unchanged, but tensile strength and Young's moduli deteriorated in modified silica filled systems in comparison with pure silica filled systems. The introduction of the organic modified silica gave a higher antibacterial activity. All nanocomposites were capable of chelating Cu (II) as well as Fe (III) at a different degree. Thus, the prepared chitosan/modified silica nanocomposites exhibited both antimicrobial and chelating properties.     

微珠析相微萃取-石墨炉原子吸收法测定岩石样品中痕量铬

采用二苯碳酰二肼为络合剂,正戊醇为萃取剂,乙醇为助溶剂,建立了微珠析相微萃取-石墨炉原子吸收法测定地质样品中痕量Cr的分析方法。实验详细探讨了微珠析相微萃取的析相条件、石墨炉原子吸收工作参数及共存离子的干扰,优化了体系萃取条件。实验结果表明：微珠析相微萃取既起到了分离富集的作用,在石墨炉升温程序中又起到了基体改进剂的作用;当萃取剂用量为0.2～1.5 mL时,使之与水完全互溶所需助溶剂体积约为水相体积的0.2～0.5倍;方法线性范围为0～10 μg·L-1,检出限为0.057 μg·L-1,相对标准偏差（RSD）为3.3%（c= 2.5 μg·L-1,n=11）;当萃取剂用量为1.5 mL、水相体积15 mL时,与直接溶液进样相比其灵敏度可提高10倍。所建立的方法用于地质标准参考物质AGV-2和G-2中Cr的测定,测定值与参考值具有较好的一致性。     

Surface hydrophobic modification of ultra-fine aluminum silicate by mechanically grinding and heating

Highly hydrophobic ultra-fine aluminum silicate can be obtained by mechanically grinding and heating both aluminum silicate particles and octadecoic acid. The results showed that the organic modifier was adsorbed on the surface of aluminum silicate particles where a little new organic group was generated, and the hydrophobicity of ultra-fine aluminum silicate powder was enhanced. Grafting reaction was mainly carried out in heating process. Due to both grinding and heating, the modifier spread on the surface of particle completely and bonded with Si to form Si-O-C, and with Al to form acyl alumina in bidentate coordination. As a result, a highly hydrophobic layer was formed on the powder surface. However, it was unsuitable for heating temperature to exceed 180 °C, or else the layer would be destroyed. All the above points represent a useful effort for surface-grafting modification of powder particles. In this study, a novel method as a reference was provided on the surface-grafting modification of powder particles.     

Effects of Modifier Concentration on Structure and Viscoelastic Properties of Copolyester/Clay Nanocomposites

Abstract

Poly(ethylene glycol‐co‐cyclohexane‐1,4‐dimethanol terephthalate)(PETG)/clay nanocomposites were prepared via melt intercalation technique. The effects of concentration of the organic modifier in the clay on the properties of the nanocomposites were studied. Three clays modified using the same alkyl ammonium modifier, but differing in modifier concentration, are used for this purpose. The nanocomposites are characterized using wide‐angle x‐ray diffraction for their structure. Dynamic mechanical analysis of these nanocomposites is also studied to investigate their viscoelastic behaviors. The x‐ray diffraction study shows an increase in the interlayer spacing of organically modified clays as compared to that of Na⁺ clay. The extent of increase in the interlayer spacing is dependent on the concentration of organic modifier used to modify the montmorillonite. The presence of well‐defined diffraction peaks and the observed increase in the interlayer spacing in the nanocomposites imply the formation of an intercalated hybrid. Dynamic mechanical properties show an increase in the storage modulus of the nanocomposite over the entire temperature range studied, as compared to the pristine polymer. Investigation of the rubbery plateau modulus confirms the reinforcing effect of organically modified clay. The observed enhancement in the modulus was greater for the clay with the lowest content of the organic modifier. These results indicate that in nanocomposites, apart from the compatibility of the organic modifier with the polymer, its concentration in the interlayer also plays a critical role in the structure development and thus in the enhancement of the properties. The nanocomposites showed reduced damping, which was governed by the modifier concentration in the clay.     

氢化物—原子荧光法测定植物及人发中的痕量硒

本文研究开发了在捕集剂覆盖下低温焙烧富集分离氢化物原子荧光光谱法测定植物和人发样品中的痕量硒，本方法克服了使用混合酸分解样品时，有机物质不能彻底分解而给测定带来的不利影响。其方法精密度和准确度均能满足测定的要求。     

Separation of Ammonium and Nitrate for Isotopic Analysis of Nitrogen 15 Using Vacuum Distillation Method

The parameters affecting the vacuum distillation method for quantitative separation of ammonium and nitrate for mass spectrometric determination of ¹⁵N were investigated. The vacuum distillation was found to be advantageous to steam distillation method because no interference from organic compounds was encountered, greater volumes could be processed and no previous evaporation of the water samples was necessary. The mass spectrometric isotopic analysis of nitrogen 15 proved the suitability of the vacuum distillation method for quantitative separation of ammonium and nitrate.     

Synthesis and Characterization of New Organic–Inorganic Hybrid Nanosilica Fillers Prepared by Sol–Gel Reaction

In light of the success of making multicomponent sol–gel glasses, in this study the synthesis of new hybrid nanosilicas with controlled hydrophilic/hydrophobic properties was carried out by incorporating organic based species with appropriate functional groups to inorganic based alkoxides by co-condensation reaction. Furthermore, in this study the acidity and the water content during reaction synthesis was proven to be critical in controlling the structure of the hybrid nanosilicas. These nanosilicas with different hydrophobicity were obtained by using TEOS (tetraethylorthosilicate) and 10 wt% two organic modifiers (tris-hydroxymethylaminomethane — TRIS — and 1,1,1,3,3,3-hexamethyldisilazane-HDMS). The average diameter of the nano-particles ranged between 7 and 10 nm. The addition of the organic modifiers changed the pH of the hybrid nanosilicas, to a different extent depending on the nature of the organic modifier. The hydrophobicity in the hybrid nanosilicas estimated from pH measurements in water and ethanol, and from IR spectroscopy, can be tailored by incorporating different organic modifiers on the network during synthesis. Finally, the measurement of pH of the hybrid nanosilicas by using solvents with different polarity/acidity was a simple and efficient method of assessing the hydrophobicity of the nanosilicas.     

析相萃取火焰原子吸收法测定矿样中的锌

非离子表面活性剂的水溶液在温度升高达到其浊点时会形成胶束相析出。文章研究了利用其浊点使待测离子的络合物富集在胶束内一起析出 ,进行析相萃取分离富集后 ,应用火焰原子吸收光谱法测定矿样中锌的新方法 ;着重讨论了采用TritonX 10 0做析相剂、正辛醇降低浊点和析出相的密度以及络合剂的选择、酸度及振荡次数的影响等析相萃取条件。方法检出限为 0 0 0 5 μg·mL-1。用于岩矿中锌的分析测定 ,结果令人满意     

时频域独立元分析方法实现超声兰姆波的多模式分离

为方便兰姆波信号分析与模式定征,提出一种将短时傅里叶变换(Short-Time Fourier Transform,STFT)与独立元分析(Independent Component Analysis,ICA)相结合的多模式超声兰姆波识别方法.首先通过STFT将兰姆波时域信号投影至时频域,基于各模式信号在时频域相对独立...