萃取催化动力学光度法测定痕量钼

研究了在pH 5 5的弱酸性介质中 ,利用钼 (Ⅵ )催化过氧化氢氧化邻氨基酚显色的指示反应 ,用萃取平衡控制反应时间和水相中邻氨基酚的浓度及反应程度 ,通过测量 42 4nm处有机相的吸光度 ,建立了萃取催化动力学光度法测定痕量钼的新方法 ,方法的线性范围为 0 0 0 5 0～ 2 0mg·L- 1 ,检出限为 2 0× 10 - 6g·L- 1 。用于豆类中钼的测定 ,结果满意     

利用协同催化效应萃取催化光度法测定痕量铬

研究了在pH 5.5的HAc-NaAc介质中,利用Fe(Ⅲ),Cr(Ⅵ)对H₂O₂氧化邻氨基酚的协同催化作用,用萃取平衡控制反应时间和水相中邻氨基酚的浓度及协同催化反应进行的程度,通过测量424 nm下有机相的吸光度,建立了协同萃取催化光度法测定铬的新方法。方法的线性范围为：0.001 0～0.90 mg·L-1,检出限为5.0×10-6g·L-1。用于自来水和废水中铬的测定,结果满意。     

以吐温-80为增溶剂催化光度法测定痕量钒(Ⅴ)

本文报道了在硫酸性介质中 ,以吐温 - 80为增溶剂 ,溴酸钾氧化姜黄催化光度法测定痕量钒 ( )的新体系。方法的检出限为 2 .6× 10 -3mg· L-1;相对标准偏差为 2 .7% (n=9) ,线性范围为 0 .0 12— 0 .0 4 0mg· L-1。可用于测定水样中痕量钒 ( ) ,结果满意     

吖啶红与铬(Ⅵ)的高灵敏度荧光反应及应用

研究了在硫酸介质中,铬(Ⅵ)氧化吖啶红荧光增强反应的最佳实验条件,建立了测定痕量铬(Ⅵ)的新的高灵敏度荧光分析法。该方法的检出限为0.6 μg·L-1,线性范围为2.0～32 μg·L-1,对含量为4.0和28 μg·L-1的Cr(Ⅵ)标准溶液进行11次平行测定, 其相对标准偏差分别为2.0%和1.0%。该法用于电镀液、废铬酸洗液及合金钢中痕量铬(Ⅵ)的测定,与标准样品和二苯碳酰二肼分光光度法进行了对照,获得了满意结果。     

微乳液增敏催化光度法测定痕量铬的研究

研究了在微乳液(溴化十六烷基三甲基胺(CTMAB)/正戊醇/正庚烷/水)介质中,痕量铬(Ⅵ)催化过氧化氢氧化茜素红的褪色反应,建立了测定痕量铬的催化动力学新方法。在微乳液体系中,方法的灵敏度比在表面活性剂CTMAB体系中提高了72.5%,催化反应的表观活化能为55.7 kJ·mol-1。水浴温度升高,灵敏度显著提高,校准曲线在不同的反应温度下线性范围不同,在80 ℃反应温度下,线性范围为2.4～75 μg·L-1,检出限达4.27×10-10g·mL-1,相对标准偏差为1.84%(n=11)。该法已应用于电镀废水中铬(Ⅵ)的测定,结果令人满意。     

粉煤灰中微量铬的光度法测定

在HNO3 介质中利用Cr2 O2 - 7氧化偶氮胂Ⅲ的褪色反应 ,对粉煤灰中的痕量铬进行测定。结果表明 ,在 3 2mol·L- 1 的硝酸介质中褪色反应具有高的灵敏度 ,反应产物的最大吸收波长为 52 0nm ,摩尔吸光系数为1 9× 1 0 6 L·mol- 1 ·cm- 1 。铬 (Ⅵ )含量在 0 0～ 40 0 μg·L- 1 范围内服从比耳定律。该法用于测定粉煤灰中的铬 ,得到了满意的结果。     

二甲苯胺蓝褪色光度法测定水中痕量铬

研究了在酸性介质中铬(Ⅵ)催化溴酸钾氧化二甲苯胺蓝褪色的最佳条件.本法λmax=515nm,表观摩尔吸光系数为2.5×104L·mol-1·cm-1,线性范围为0-26μg/25mL.用于水样中痕量铬的测定,结果令人满意.     

吡咯红Y-过氧化氢-铬(Ⅵ)体系催化荧光法测定痕量铬(Ⅵ)

在HAc-NaAc缓冲体系中,痕量铬(Ⅵ)对过氧化氢氧化吡咯红Y的氧化还原反应有催化作用,使吡咯红Y荧光减弱,据此建立了催化荧光法测定痕量铬(Ⅵ)的新方法,同时考察了该催化反应的最优条件及动力学性质.该方法的表观活化能为159.92 kJ·mol-1,反应速率常量为5.7×10-2s-1,检测限为0.012μg·mL-1,测定线性范围为0.02～0.24 μg·mL-1.该方法用于对河水、工业废水及电镀废水中铬(Ⅵ)的测定,结果令人满意.     

萃取动力学光谱法测定癌组织中的微量元素

本文研究了在 p H9.2～ 9.5氨性缓冲溶液中 ,Cu( )催化 H2 O2 氧化溴酚蓝和丁基罗丹明 B等色染料离子对褪色的新指示反应 ,建立了较为广泛的快速终止催化反应的新方法。本方法测定铜 ,灵敏度为 0 .0 2μg·L- 1 ,线性范围为 0 .1～ 10 μg· L- 1。用于直肠癌组织中微量元素铜的测定 ,结果满意     

催化动力学光度法测定抗癌中草药中痕量硒Ⅰ．溴酸钾一罗丹明B体系

研究了硝酸介质中痕量硒(Ⅳ)催化溴酸钾氧化罗丹明B的褪色反应及动力学条件, 建立了动力学光度法测定痕量硒(Ⅳ)的新方法, 其灵敏度为0.905 μg·L-1, 测定范围0～9.6 μg*L-1. 用于测定抗癌中草药中的硒(Ⅳ), 获得了满意的结果.     

Film morphology and orientation of amino silicone adsorbed onto cellulose substrate

A series of amino silicones with different amino values were synthesized and adsorbed onto surfaces of cotton fibers and cellulose substrates. The film morphology, hydrophobic properties and surface composition of the silicones are investigated and characterized by field emission scanning electron microscope (FESEM), atomic force microscope (AFM), contact angle measurement, X-ray photoelectron spectroscopy (XPS) and attenuated total reflectance infrared (ATR-IR). The results of the experiments indicate that the amino silicone can form a hydrophobic film on both cotton fibers and cellulose substrates and reduce the surface roughness significantly. Furthermore, the roughness becomes smaller with an increase in the amino value. All these results suggest that the orientation of amino silicone molecule is with the amino functional groups of amino silicone molecule adsorbed onto the cellulose interface while the main polymer chains and the hydrophobic Si-CH₃ groups extend toward the air.     

Adsorption of amino acids on indium arsenide (1 0 0) surfaces: Assessment of passivation capabilities

Angle-Resolved X-ray Photoelectron Spectroscopy (ARXPS) was used to examine amino acid bonding and oxide removal on InAs(1 0 0) surfaces. Five amino acids were studied, including cysteine, lysine, aspartic acid, glutamic acid and arginine. Observations on the ability of specific functional groups to prevent oxide formation were made by examining the thickness of oxide films on the functionalize surfaces. Amino acids that possessed more than one functional group having resonance were shown to most effectively affect oxide formation. The influence of these groups on the electronic structure of InAs(1 0 0) provides insight into how multifunctional passivation strategies could be beneficial, as well as showing how biological molecules might affect detection when InAs(1 0 0) is used as a platform.     

UPLC测定烟叶中的氨基酸含量

采用UPLC法测定烟叶中氨基酸的含量。Waters Acquity UPLC BEH C18色谱柱(2.1mm×100mm,1.7μm),AccQ.Tag Ultraa Eluent A及AccQ.Tag Ultraa Eluent B梯度洗脱,流速为0.7mL·min-1,波长:248nm,柱温55℃。18种氨基酸在0.0030-0.204mg/mL范围内有良好的线性关系(r0.9994),平均回收率(n=6)为98.7%。该方法10min内18种氨基酸可完全分离且具有快速、准确、重复性好的特点。     

Vibrational Spectroscopic and Theoretical Studies of Urea Derivatives with Biochemical Interest: N,N′-Dimethylurea,N,N,N′,N′-Tetramethylurea,and N,N′-Dimethylpropyleneurea

Abstract

Mid-infrared, far-infrared, and Raman vibrational spectroscopic studies were combined with density functional theory (DFT) calculations and normal coordinate force field analyses for N,N′-dimethylurea (DMU), N,N,N′,N′-tetramethylurea (TMU), and N,N′-dimethylpropyleneurea (DMPU: IUPAC name 1,3-dimethyltetrahydropyrimidin-2(1H)-one). The equilibrium molecular geometry of DMU (all three conformers), TMU, and DMPU and the frequencies, intensities, and depolarization ratios of their fundamental infrared (IR) and Raman vibrational transitions were obtained by DFT calculations. The vibrational spectra were fully analyzed by normal coordinate methods as well. A starting force field for DMPU was obtained by adapting corresponding force constants for DMU and TMU, resulting after refinements in the stretching force constants C=O (7.69, 7.30, 7.68 N·cm^?1), C–N (5.16, 5.55, 5.05 N·cm^?1), and C-Me (5.93, 4.00, 4.22 N·cm^?1) for DMU, TMU, and DMPU, respectively. The dominating conformer of liquid DMU was identified as trans-trans, strong intermolecular hydrogen bonding was verified in solid DMU, and weak dipole–dipole association was found in liquid TMU and in DMPU. Special attention was paid to analyzing the methyl group frequencies, which revealed deviations from local C_3v symmetry. A linear correlation was found between the CH stretching force constants and the inverse of the CH bond lengths (1/r ²). The averaged NH stretching frequencies of gaseous, dissolved, and solid urea and of DMU, with variations for hydrogen bonding of different strength, are linearly correlated to the NH stretching force constants. Characteristic skeletal vibrations were assigned for a broad variety of urea derivatives and also for pyrimidine derivatives, which all contain the N₂C=O entity. The very strong IR bands of C=O stretching (1,676 ± 40 cm^?1) and asymmetric CN₂ stretching (1,478 ± 60 cm^?1), and the very intense Raman feature of symmetric CN₂ stretching or ring breathing (757 ± 80 cm^?1), can be recognized as fingerprint bands also for the pyrimidine derivatives cytosine, thymine, and uracil, which all are nucleobases in DNA and RNA nucleotides.     

近红外分析技术在食品氨基酸检测中应用的研究进展

综述了近红外分析技术在农作物生长及食品加工处理过程中氨基酸检测的应用情况,及其研究进展。对近红外分析食品氨基酸应用中涉及的化学值HPLC检测以及化学计量学方法进行总结,对相关原始文献中的数据、资料和主要观点进行整理和归纳。对氨基酸的HPLC、化学计量学分析方法及其在农作物品质监测、茶叶中氨基酸和茶多酚含量的同时测定、饲料品质鉴定、奶酪火腿肉制品中氨基酸及其他化学成分含量的测定情况进行了综述,分析了方法的优缺点并对近红外分析技术在食品氨基酸检测中应用进行了展望。近红外光谱在氨基酸检测中应用的发展需基于氨基酸高效液相色谱检测的化学值来建立相应的模型,模型传递的问题是目前制约其大范围推广的主要原因。在线分析可以监测从原料到产品的整个反应变化过程,满足食品从生产到销售等领域中品质实时监控的需求,将是今后重要的发展方向。     

斑头雁不同组织氨基酸的组成和含量分析

采用高效液相色谱法对斑头雁卵、肌肉和羽毛中17种氨基酸进行了含量的测定,并分析其中必需氨基酸的含量,为斑头雁的保护和利用提供依据。结果表明,斑头雁的卵、腿肌、胸肌和羽毛中均含有17种氨基酸,必需氨基酸含量较高,配比合理,有较高的营养价值。     

PLS分光光度法同时测定混合氨基酸

本文将偏最小二乘法(PLS)用于分光光度法同时测定混合氨基酸体系中的苯丙氨酸、色氨酸和酪氨酸.对校准样品集的实验设计及测量波长点的选择等进行了实验和讨论,并与最小二乘法、卡尔曼滤波法和因子分析法的计算结果进行了对比,PLS法的计算结果最精确,偏差最小.由此可见,PLS法对于这类组分间存在相互作用的样品的测定是一种简捷、准确的多组分同时测定方法,通过校准集来校正相互作用带来的影响,是PLS法偏差最小的原因.     

CdTe纳米棒的合成和性质

用半胱氨酸和巯基乙酸的混合配体作为修饰剂制备了高发光水溶性CdTe纳米棒,同时研究了CdTe纳米棒与高半胱氨酸,酪氨酸,脯氨酸,半胱氨酸,胱氨酸等5种氨基酸之间的相互作用,实验发现CdTe纳米棒纵横比和光致发光可以由回流时间来控制.     

Kalman滤波荧光光度法同时测定酪氨酸、色氨酸和苯丙氨酸

苯丙氨酸的荧光峰完全包含在酪氨酸荧光峰之中，酪氨酸和色氨酸的荧光峰也严重重叠。用卡尔曼滤波法解析该体系给出了令人满意的分析结果。回收率为９４．０～１０５％，相对标准偏差不大于３．６％（个别一点除外）。将试剂空白作为一个组分计算，从而免去了试剂空白扣不准给分析结果带来的影响。利用新息序列的白噪音特性来判断结果的可靠性。     

新疆6种红景天属植物中微量元素和氨基酸含量分析

测定新疆6种红景天属植物的根及根茎中微量元素Na,K,Mg,Ca,Mn,Fe,Cu,Zn,Se和20种氨基酸含量,结果表明,9种微量元素在6种红景天根及根茎中含量中不同,6种红景天根及根茎中分别含有8－18种氨基酸,其中人体必需氨基酸3－7种。