6291型热变形温度和维卡软化温度测试仪的校准及故障排除

介绍6291型热变形温度和维卡软化温度测试仪的温度校准和位移校准方法，对测试仪的一些常见故障，例如电源故障，主温度传感器故障，电加热系统控制单元故障及测试站的温度偏差较大等进行了分析，并给出了排除故障的方法。     

Voltammetric Detection of Free Sulfhydryl Compounds in Food Flours

Cyclic voltammetry has been applied to the rapid measurement of free SH‐compounds in food flours samples. The protocol is based on the electrochemical adaptation of the Ellman's test, where the DTNB reacts with SH‐compounds present in food flour extracts, resulting in the equimolar production of the electroactive compound TNBA which, in turns, reacts with phenylendiamine. The reaction is found to provide an analytical signal from which to quantify indirectly free sulfhydryl compounds in flours extracts.     

On-line testing of gas chromatographic columns with a programmable computing integrator

Summary A program is described which calculates the number of effective plates and the coating efficiency over the entire range of a test chromatogram. The peak widths at half height are derived by assuming a Gaussian peak shape. The interpolated peak width at k=4 is used for computing a standardized number of effective plates. Plate height, column permeability, overall performance and a novel parameter called sampling efficiency are calculated from 5 other figures — i. e. carrier gas code, pressure drop, column length, column temperature and particle size.Dedicated to Dr. Leslie S. Ettre for his 60th birthday.     

密胺-脲甲醛树脂合成工艺放大研究

以密胺－脲甲醛树脂合成的小试工艺条件为依据，完成了放大试验过程的工艺研究。研究结果与小试研究的工艺条件相吻合。     

An optical surface plasmon resonance biosensor for determination of tetanus toxin

Surface plasmon resonance (SPR) has been successfully applied for the simple, rapid, and label-free assay of various biomolecules. This assay evaluates a novel wavelength modulation SPR biosensor for the detection of tetanus toxin. The wavelength modulation SPR biosensor is designed based on fixing the incident angle of light and measuring the reflected intensities in the resonance wavelength range spanning 400-800 nm simultaneously. Tetanus toxin (TeNT), one of the most potent toxins known, is synthesized as a 150 kDa single polypeptide chain. The SPR biosensor has been shown to be capable of directly detecting concentration of tetanus toxin as low as 0.028 Lf ml⁻¹. Under selected experimental conditions, the SPR biosensor has a good reproducibility, sensitivity and reversibility. The results illustrate how wavelength modulation SPR biosensor can be used to detect biomolecular interactions.     

钒氧阴离子团簇与小分子碳氢化合物反应的实验和理论研究

为了在分子层次上揭示相关催化反应的机理, 人们对过渡金属氧化物团簇与碳氢化合物分子反应进行了大量研究. 相比于过渡金属氧化物团簇阳离子, 阴离子对一些碳氢化合物的活性弱得多, 因此研究还很少. 在本工作中, 我们通过激光溅射产生钒氧团簇阴离子VxOy, 产生的团簇在接近热碰撞条件下与烷烃(C2H6和C4H10)以及烯烃(C2H4和C3H6) 在一个快速流动反应管中进行反应, 飞行时间质谱用来检测反应前后的团簇分布. 在VxOy与烷烃的反应中, 生成了产物V2O6H-和V4O11H-; 在与烯烃的反应中, 产生了相应的吸附产物V4O11X-(X=C2H4或C3H6). 密度泛函理论计算表明: V2O-6和V4O-11可以活化烷烃(C2H6和C4H10)的C—H键, 也可以与烯烃(C2H4和C3H6)发生3+2环化加成反应形成一个五元环结构(-V-O-C-C-O-), C—H键活化与环加成反应都需经历可以克服的反应能垒. 理论计算与实验观测结果相符合. V2O-6和V4O-11团簇都具有氧原子自由基(O·或O-)的成键特征, 活性O-物种也经常出现在钒氧催化剂表面, 因而本研究在分子水平上, 揭示了表面活性氧物种与碳氢化合物反应的机理.     

液相色谱/大气压化学电离飞行时间质谱分析氢化可的松中微量杂质

采用液相色谱/大气压化学电离飞行时间质谱测定氢化可的松对照品中微量杂 质，并采用源内碰撞诱导解离质谱进行了结构定性分析。方法简单，可靠，重现性 好。     

Protein secondary structure and stability determined by combining exoproteolysis and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

In the post-genomic era, several projects focused on the massive experimental resolution of the three-dimensional structures of all the proteins of different organisms have been initiated. Simultaneously, significant progress has been made in the ab initio prediction of protein three-dimensional structure. One of the keys to the success of such a prediction is the use of local information (i.e. secondary structure). Here we describe a new limited proteolysis methodology, based on the use of unspecific exoproteases coupled with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), to map quickly secondary structure elements of a protein from both ends, the N- and C-termini. We show that the proteolytic patterns (mass spectra series) obtained can be interpreted in the light of the conformation and local stability of the analyzed proteins, a direct correlation being observed between the predicted and the experimentally derived protein secondary structure. Further, this methodology can be easily applied to check rapidly the folding state of a protein and characterize mutational effects on protein conformation and stability. Moreover, given global stability information, this methodology allows one to locate the protein regions of increased or decreased conformational stability. All of this can be done with a small fraction of the amount of protein required by most of the other methods for conformational analysis. Thus limited exoproteolysis, together with MALDI-TOF MS, can be a useful tool to achieve quickly the elucidation of protein structure and stability.     

钒氧阴离子团簇与小分子碳氢化合物反应的实验和理论研究

为了在分子层次上揭示相关催化反应的机理, 人们对过渡金属氧化物团簇与碳氢化合物分子反应进行了大量研究. 相比于过渡金属氧化物团簇阳离子, 阴离子对一些碳氢化合物的活性弱得多, 因此研究还很少. 在本工作中, 我们通过激光溅射产生钒氧团簇阴离子VxOy, 产生的团簇在接近热碰撞条件下与烷烃(C2H6和C4H10)以及烯烃(C2H4和C3H6) 在一个快速流动反应管中进行反应, 飞行时间质谱用来检测反应前后的团簇分布. 在VxOy与烷烃的反应中, 生成了产物V2O6H-和V4O11H-; 在与烯烃的反应中, 产生了相应的吸附产物V4O11X-(X=C2H4或C3H6). 密度泛函理论计算表明: V2O-6和V4O-11可以活化烷烃(C2H6和C4H10)的C—H键, 也可以与烯烃(C2H4和C3H6)发生3+2环化加成反应形成一个五元环结构(-V-O-C-C-O-), C—H键活化与环加成反应都需经历可以克服的反应能垒. 理论计算与实验观测结果相符合. V2O-6和V4O-11团簇都具有氧原子自由基(O·或O-)的成键特征, 活性O-物种也经常出现在钒氧催化剂表面, 因而本研究在分子水平上, 揭示了表面活性氧物种与碳氢化合物反应的机理.     

超临界流体萃取仪器的研制

本文报道了以国产原配件为基础，成功地研制了分析规模的超临界流体萃取仪器、并对仪器性能进行了全面考察，仪器性能稳定，重现性良好（ＲＳＤ＜３．１％），定量线性关系可靠，可满足定量萃取的要求。