质谱在肽和蛋白质序列分析中的应用

了解肽和蛋白质的序列对理解其功能具有重要意义，测定其序列也是当前生命 科学研究中的重要内容之一，质谱作为高灵敏度的测定分子结构的仪器，其高灵敏 度、广泛的适用性及快速性等特性使它具有很大潜力发展成为辅助传统测序方法的 新方法，并得到了广泛的关注。从离子活化方法（包括碰撞诱导解离CID、源后裂 解PSD、源内裂解ISD等）、衍生化作用以及氨基酸残基消除方式（高能活化产生亚 稳离子、化学降解、酶降解）等多个角度介绍了利用质谱分析多肽和蛋白质序列的 方法，并对其发展前景作出展望。     

ⅥB族金属叁键有机化合物的研究进展

本文对一类重要的ⅥB族金属叁键化合物R_2M_2(CO)_4(R为环戊二烯基及类环戊二烯基)近年来的研究成果进行了综述,综述重点是这类化合物的官能团M≡M参键的化学活性,全文包括R_2M_2(CO)_4的合成及结构,M≡M叁键与亲核试剂、与碳-碳重键,与氧或与金属羰基物等试剂的反应及其应用。     

Xylanolytic enzyme production by anAspergillus niger isolate

Production of xylanolytic enzymes by anAspergillus niger CCMI 850 isolate was investigated in batch cultures. The effect of the composition of a fermentation medium that did not include chemical inducers, on β-xylanase, β-xylosidase, α-l-arabinofuranosidase, and total cellulase activity was studied. With 4% xylan as the carbon source, about 65 U/mL of β-xylanase was obtained, whereas the total cellulase activity was undetectable, under the specified conditions. This β-xylanase activity represents the highest reported for a wild-type strain ofA. niger. The effect of pH and temperature on the activity of β-xylanase was studied. Partial characterization of the β-xylanase showed that with insoluble birchwood as substrate theK _m andV _max were 0.3 mM and 19 μmol/min, respectively. Aspects of using the crude β-xylanase preparation for applications in the pulp and paper industry were discussed.     

Darstellung und Strukturen einiger N-(Tri-t-butoxysilyl)anilin-Derivate

Formation and Structures of N-(tri-t-butoxysilyl)aniline Compounds Para-substituted N-(tri-t-butoxysilyl)anilines (t-BuO)₃SiNRC₄H₄X-p, R = H, CH₃, with substituents of high electron affinity (X = CN, NO₂) were prepared by a one-pot reaction of tri-t-butoxychlorsilane, potassium t-butanolate and substituted anilines. Corresponding compounds with substituents of low electron affinity (X = OMe, H) preferably were prepared by metalation of anilines with sodium amide. Four crystal structures were determined. N-(tri-t-butoxysilyl)-p-nitro-aniline, N-methyl-(N-tri-t-butoxysilyl)-p-nitroaniline and N-(tri-t-butoxysilyl)-p-cyanoaniline crystallize at 298 K monoclinically, N-(tri-t-butoxysilyl)aniline crystallizes orthorhombically.     

Advances in two-dimensional GC with glass capillary columns

A versatile two-dimensional gas chromatograph is described, consisting of 2 separate ovens, one intermediate trap, an auxiliary inlet, and the necessary hardware to effect off-line switching according to the principle of Deans. The unit has been designed for use with high resolution glass capillary columns. The performance of individual instrumental components was critically evaluated. Results showed that low dead volume glass to metal connections were required in the manifold and detector lines to minimize extra-column effects. The mass of the intermediate trap must be low to allow rapid heating. Operational parameters are discussed and examples of some applications are shown.     

Size Dependence of Electronic Excitation Energy in Linear C_(2n)H and C_(2n-1)N

IntroductionCarbon chains are among the most attractivecandidates as the carriers of the diffuse interstellarbands ( DIBs) [1] .To detect the carbon chains indark clouds and carbon stars[2 ] ,itis very importantto understand their electronic spectra.Maier andhis coworkers have measured the polyacetylenicradicals C2 n H( n=1— 4) and C2 n-1H( n=2— 6) bythe rotational spectroscopy[3 ,4] and the species n≤ 4have been detected in dark interstellar clouds[5,6] .In neon matrices,the B2 Π← X2…     

无焰燃烧烟密度标准物质的研制

介绍无焰燃烧烟密度标准物质的研制方法。选用合适的α-纤维素作为原材料,经打浆造纸后,作为标准物质候选物,经均匀性检验和稳定性考察合格后,对标准物质进行定值。在无焰燃烧条件下烟密度标准物质的标准值为175,扩展不确定度为8;校正烟密度标准物质的标准值为166,扩展不确定度为8。     

Comparison of slurry sampling and microwave-assisted digestion for calcium, magnesium, iron, copper and zinc determination in fish tissue samples by flame atomic absorption spectrometry

The development of a slurry sampling method for the determination of calcium, copper, iron, magnesium and zinc in fish tissue samples by flame atomic absorption spectrometry is described. In comparison with microwave-assisted digestion, the proposed method is simple, requires short time and eliminates total sample dissolution before analysis. Suspension medium was optimized for each analyte to obtain quantitative recoveries from fish tissue samples without matrix interferences. Nevertheless, iron recoveries higher than 46% were not found. Treatment of samples slurried in nitric acid by microwave irradiation for 15-30 s at 75-285 W permitted to achieve efficient recoveries for calcium, iron, magnesium and zinc. Further improvement in the matrix effects for iron determination was accomplished by the use of an additional step of short microwave-assisted suspension treatment. However, standard addition method was required for calcium and copper determination, being necessary hydrochloric acid as suspension medium for the last one. Although copper could not be determined in the certified reference material using microwave-assisted digestion, the accuracy of the slurry sampling method was verified for all the investigated analytes. Detection limits were 22.8 ± 8.0, 0.884 ± 0.092, 5.07 ± 0.76, 35.5 ± 0.7 and 1.17 ± 0.04 μg g⁻¹ for calcium, copper, iron, magnesium and zinc, respectively. The standard deviations obtained using slurry sampling method and microwave-assisted digestion were not significantly different, and the mean relative standard deviation of the over-all method (n = 3) of the slurry sampling method for different concentration levels was below 12%.     

Gas Chromatographic Method for Routine Determination of Oleanolic and Ursolic Acids in Medicinal Plants

Summary A rapid and simple gas chromatographic method has been established for routine analysis of free oleanolic and ursolic acids in dried samples of medicinal herbs. Soxhlet extraction of triterpenes was followed by solid-phase extraction (SPE). Amounts of the compounds were measured by gas chromatography after silylation of the purified samples. Experiments were performed to establish the optimum conditions (e.g. solvent, and mode and duration of extraction) for calibration curve linearity, sensitivity, reproducibility, and recovery. The conditions used for derivatization and gas chromatographic analysis resulted in an improvement on literature data. The method devised enables accurate routine measurement of many samples in quite a short time (e.g. for chemotaxonomical screening, or quality control of herbal drugs). The practical application of the method was illustrated on five Lamiaceae species.     

Synthesis and Structure of 1- and 2-Isomers of (Trimethoxysilylmethyl) and (Silatranylmethyl)benzotriazole

We have synthesized 1- and 2-(trimethylsilylmethyl)- and 1- and 2-(trimethoxysilylmethyl)benzotriazoles by reaction of 1,2,3-benzotriazolylsodium with trimethyl- or trimethoxy(chloromethyl)silane. We obtained 1- and 2-(silatranylmethyl)benzotriazoles by transesterification of the latter with triethanolamine.