白眉蝮蛇蛇毒和蛇毒酶的基质辅助激光解吸电离飞行时间质谱法研究

应用基质辅激光解吸电离飞行时间质谱（ＭＡＬＤＩ－ＴＯＦ－ＭＳ）法对长白山眉蝮蛇蛇毒和纯化得到的两种蛇毒酶进行了研究,得到了它们的分子质量并验证了纯度。同时还考察了不同产地的蛇毒、蛇毒蛋白浓度以及基质对分析结果的影响,实验结果表明ＭＡＬＤＩ－ＴＯＦ－ＭＳ法是检测蛋白纯化过程和分析蛋白相对分子质量十分有效的手段。     

应用激光解吸质谱和十二烷基硫酸钠—聚丙烯酰胺凝胶电泳分析蛇毒？…

应用基质辅助激光解吸电离飞行时间质谱（ＭＡＬＤＩ－ＴＯＦ－ＭＳ）和ＳＤＳ－聚丙烯酰胺凝胶电流对吉林省两地市的同种白眉蝮蛇蛇毒中具有抗栓塞药效的精氨酸酯酶进行了分析了分析和比较。ＭＡＬＤＩ－ＴＯＦ－ＭＳ法具有快速、准确度高、灵敏度高的优点,两种方法结合,互为补充,取得了令人满意的结果。ＭＡＬＤＩ－ＴＯＦ－ＭＳ完全可以直接用作蛇毒成分分离过程中重要的研究手段。     

MALDI－TOF－MS法分析人血清白蛋白

用基质辅助激光解吸附飞行时间质谱（ＭＡＬＤＩ－ＴＯＦ－ＭＳ）法分析测定了人血清白蛋白。结果表明，全军血液制品研究中心应用Ｒｉｖａｎｏｌ和Ｃｏｈｎ＇ｓ两种方法分离提取的人血清白蛋白，其分子量与理论计算值相吻合，其纯度与市售标准人血清白蛋白相一致，用ＭＡＬＤＩ－ＴＯＦ－ＭＳ法分析鉴定人血清白蛋白，准确、简便和灵敏（仅需ＰＭ浓度样品），且重复性好，日内和日间差的变异系数均小于０．０３％，是ＳＤＳ－ＰＡＧＥ电泳法所无法比拟的。     

ONE－POT STEREOSELECTIVE SYNTHESIS OF FUSED RING SYSTEMS CONSISTING OF ISOXAZOLINE AND TETRAHYDRO－FURAN，－THIOPHENE，OR－PYRROLE VIA INTRAMOLECULAR CYCLOADDITION OF SILYL NITRONATES DERIVED FROM α－NITROALKENES

ＯＮＥ－ＰＯＴＳＴＥＲＥＯＳＥＬＥＣＴＩＶＥＳＹＮＴＨＥＳＩＳＯＦＦＵＳＥＤＲＩＮＧＳＹＳＴＥＭＳＣＯＮＳＩＳＴＩＮＧＯＦＩＳＯＸＡＺＯＬＩＮＥＡＮＤＴＥＴＲＡＨＹＤＲＯ－ＦＵＲＡＮ，－ＴＨＩＯＰＨＥＮＥ，ＯＲ－ＰＹＲＲＯＬＥＶＩＡＩＮＴＲＡＭＯＬＥ...     

α-AMIDOALKYLATION VIA SULFONES:TOWARDS THE SYNTHESIS OF ANT VENOM ALKALOIDS

α－ＡＭＩＤＯＡＬＫＹＬＡＴＩＯＮ　ＶＩＡ　ＳＵＬＦＯＮＥＳ：ＴＯＷＡＲＤＳ　ＴＨＥ　ＳＹＮＴＨＥＳＩＳ　ＯＦ　ＡＮＴ　ＶＥＮＯＭ　ＡＬＫＡＬＯＩＤＳα－ＡＭＩＤＯＡＬＫＹＬＡＴＩＯＮＶＩＡＳＵＬＦＯＮＥＳ：ＴＯＷＡＲＤＳＴＨＥＳＹＮＴＨＥＳＩＳＯＦ...     

INDIRECT THERMO－OPTICAL DETECTION FOR CAPILLARY ELECTROPHORESIS SEPARATION OF AMINO ACIDS

ＩＮＤＩＲＥＣＴ　ＴＨＥＲＭＯ－ＯＰＴＩＣＡＬ　ＤＥＴＥＣＴＩＯＮ　ＦＯＲ　ＣＡＰＩＬＬＡＲＹ　ＥＬＥＣＴＲＯＰＨＯＲＥＳＩＳ　ＳＥＰＡＲＡＴＩＯＮ　ＯＦ　ＡＭＩＮＯ　ＡＣＩＤＳＩＮＤＩＲＥＣＴＴＨＥＲＭＯ－ＯＰＴＩＣＡＬＤＥＴＥＣＴＩＯＮＦＯＲＣＡ...     

PARAMAGNETIC AND DIAMAGNETIC DICOPPER（Ⅱ） COMPLEXES WITH DI－SCHIFF BASE DERIVED FROM 2－HYDROXY－1－NAPHTHALDEHYDE AND1，3－DIANINO－2－PROPANOL

ＰＡＲＡＭＡＧＮＥＴＩＣＡＮＤＤＩＡＭＡＧＮＥＴＩＣＤＩＣＯＰＰＥＲ（Ⅱ）ＣＯＭＰＬＥＸＥＳＷＩＴＨＤＩ－ＳＣＨＩＦＦＢＡＳＥＤＥＲＩＶＥＤＦＲＯＭ２－ＨＹＤＲＯＸＹ－１－ＮＡＰＨＴＨＡＬＤＥＨＹＤＥＡＮＤ１，３－ＤＩＡＮＩＮＯ－２－ＰＲＯＰＡＮＯＬ...     

ZEOLITE－CATALYZED FRIEDEL－CRAFTS ACYLATION OF AROMATICS：I》．SYNTHESIS OF 4－ACYL ANISOLE WITH A HY CATALYST

ＺＥＯＬＩＴＥ－ＣＡＴＡＬＹＺＥＤＦＲＩＥＤＥＬ－ＣＲＡＦＴＳＡＣＹＬＡＴＩＯＮＯＦＡＲＯＭＡＴＩＣＳ：Ｉ．ＳＹＮＴＨＥＳＩＳＯＦ４－ＡＣＹＬＡＮＩＳＯＬＥＷＩＴＨＡＨＹＣＡＴＡＬＹＳＴ￥ＱｉＬｏｎｇＷＡＮＧ；ＹｕＤａｏＭＡ；ＸｉｎｇＤｏｎｇＪＩ；Ｈ...     

SYNTHESIS OF POLYSUBSTITUTED AROMATIC COMPOUNDS 3.THE DIELS-ALDER REACTION OF PHENYLSELENO SUBSTITUTED DIENES WITH DIMETHYL ACETYLENEDICARBOXYLATE

ＳＹＮＴＨＥＳＩＳ　ＯＦ　ＰＯＬＹＳＵＢＳＴＩＴＵＴＥＤ　ＡＲＯＭＡＴＩＣ　ＣＯＭＰＯＵＮＤＳ　３．ＴＨＥ　ＤＩＥＬＳ－ＡＬＤＥＲ　ＲＥＡＣＴＩＯＮ　ＯＦ　ＰＨＥＮＹＬＳＥＬＥＮＯ　ＳＵＢＳＴＩＴＵＴＥＤ　ＤＩＥＮＥＳ　ＷＩＴＨ　ＤＩＭＥＴＨＹＬ　Ａ...     

A NOVEL CYCLODIMERIZATION OF α，β－ UNSATURATED KETONES PROMOTED BY LOW－VALENT TITANIUM

Ａ ＮＯＶＥＬ ＣＹＣＬＯＤＩＭＥＲＩＺＡＴＩＯＮ ＯＦ α，β－ＵＮＳＡＴＵＲＡＴＥＤ ＫＥＴＯＮＥＳ ＰＲＯＭＯＴＥＤ ＢＹ ＬＯＷ－ＶＡＬＥＮＴ ＴＩＴＡＮＩＵＭ￥ＬｏｎｇＨｕＺＨＯＵ；ＧｕｉＹｕａｎＤＡＩ；ＤａＱｉｎｇＳＨＩ（Ｄｅｐａｒｔｍｅ...     

应用激光解吸质谱和十二烷基硫酸钠-聚丙烯酰胺凝胶电泳分析蛇毒精氨酸酯酶的纯度和分子量

应用基质辅助激光解吸电离飞行时间质谱(MALDI-TOF-MS)和SDS-聚丙烯酰胺凝胶电泳对吉林省两地市的同种白眉蝮蛇蛇毒中具有抗栓塞药效的精氨酸酯酶进行了分析和比较。MALDI-TOF-MS法具有快速、准确度高、灵敏度高的优点,两种方法结合,互为补充,取得了令人满意的结果,MALDI-TOF-MS完全可以直接用作蛇毒成分分离过程中重要的研究手段。     

四(对-乙酰氧醚-10-羟基喜树碱)苯基卟啉的合成及结构表征

设计并合成了一种卟啉类光敏剂与抗癌药羟基喜树碱通过共价键相连的四(对-乙酰氧醚-10-羟基喜树碱)苯基卟啉化合物. 通过紫外光谱、 红外光谱、 核磁氢谱和质谱分析等手段对其结构进行了表征. 在癌症治疗过程中目标化合物中2种药物可能起到一定的协同效应.     

Analysis of long-chain polyprenols using supercritical fluid chromatography and matrix-assisted laser desorption ionization time-of-flight mass spectrometry

The separation of long-chain polyprenols was successfully achieved using supercritical fluid chromatography (SFC). Each 100-mer greater component was separated using tetrahydrofuran as a mobile phase modifier. The molecular mass distributions derived from SFC analyses agreed with the results of matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) analyses. The number-average molecular mass calculated by MALDI-TOF-MS data were also in accord with the results of quantitative 1H-NMR analysis of terminal groups. A combination of SFC and MALDI-TOF-MS analyses is a powerful tool for the elucidation of the complicated structures of natural polyprenols.     

寡糖衍生化及基质辅助激光解吸电离飞行时间质谱分析方法研究

为提高中性寡糖在基质辅助激光解吸电离飞行时间质谱(MALDI-TOF)中的检测灵敏度,建立了以1-(4-氰基苯基)-4-哌啶碳酰肼(CPH)为衍生化试剂对寡糖的标记方法。寡糖的还原端与CPH的酰肼基团反应生成腙,使得寡糖被CPH标记,衍生物以MALDI-TOF质谱进行分析。结果表明:在反应温度95℃,醋酸浓度为0.125%(V/V),CPH过量100倍的条件下,衍生产率可达最大,并且CPH衍生可使中性寡糖在MALDI-TOF质谱中的检测灵敏度提高10倍。本方法简便快速,灵敏度高,适合微量寡糖链的质谱分析。     

小分子表面活性剂在胶内酶切增效中的应用

本研究成功地将一种有机小分子表面活性剂RapiGest SF(Waters)用于改进电泳分离的蛋白质的鉴定效率。通过基质辅助激光解析电离飞行时间质谱(MALDI-TOF-MS)的肽质量指纹谱,考察了酶切时间、加入量、加样次序、点靶方法对方法灵敏度、蛋白质鉴定率的影响。RapiGest SF浓度为0.5%~1%,在酶切之前加入可获得更多的肽段峰和更高的鉴定率。本方法考染体系的总灵敏度为332fmol,银染体系为664fmol。比较了RapiGest SF与MALDI-TOF-MS和电喷雾质谱(ESI-MS)兼容性,未观察到明显的负影响。方法操作简便,重复性较好,适合鉴定电泳分离的低丰度蛋白质。     

基质辅助激光解吸与离子化时间飞行质谱在高分子研究中的应用

对基质辅助激光解吸与离子化时间飞行质谱的发展历程和基本原理作了简要介绍,对这一分析技术在高分子研究中的应用进行了全面的综述和展望。本文表明,ＭＡＬＤＩ－ＴＯＦ－ＭＳ能快速准确地测定窄分布高分子的分子量,可测分子是一达１５０００００,所得平均分子量值及分子量分布指数与ＧＰＣ等常规方法相符;能用于高分子末端基的检测,从而推断聚合反应机理;也能用于共聚反应与共聚物结构的分析;另外,还能从分子量分布理到自     

芳香环状聚酯二聚体的结构表征

通过基质辅助激光解析电离飞行时间质谱以及核磁共振技术对芳香环状聚酯二聚体的结构进行了表征.质谱分析结果发现除了目标化合物的质子化分子离子峰外,未出现更多的碎片峰,而核磁共振结果对芳香环状齐聚物的氢以及碳的位置给予了确认.从而为芳香环状齐聚物的结构分析提供了一种新的分析方法.     

NH_4Y_3F_(10)多孔纳米晶的制备及其在MALDI-TOF-MS中的应用(英文)

利用水热法合成出NH4Y3F10多孔纳米晶。由于Y3+离子的激发态能量可以转移给具有较高振动能的有机分子,因此这些多孔纳米晶可以作为基质辅助激光解析电离飞行时间质谱的基体材料,用于检测小分子和聚乙二醇。通过与商品化的基体材料(CHCA、DHB)对比,证明NH4Y3F10多孔纳米晶是一种性能优异的基体材料。这种新型基体材料已经成功应用于有机分子、小肽、C60、缺氧诱导因子(HIFs)和聚乙二醇的分子量的检测,显示出这种基体材料具有广泛的应用前景。     

Semiconductor cadmium sulphide nanoparticles as matrices for peptides and as co-matrices for the analysis of large proteins in matrix-assisted laser desorption/ionization reflectron and linear time-of-flight mass spectrometry

The use of semiconductor cadmium sulphide nanoparticles (CdS NPs) capped with 4-aminothiophenol (ATP) and 11-mercaptoundecanoic acid (MUA) is described for the first time as matrices and as co-matrices for the analysis of peptides and proteins in matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). UV-visible spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were applied for the characterization of functionalized CdS NPs. The synthesized CdS-ATP and CdS-MUA NPs exhibit uniform size distribution with diameter of 15-25 nm and 20-30 nm, respectively. The -NH(2) (ATP) and -COOH (MUA) groups modified on the surfaces of CdS NPs provide ionizable moieties for efficient transfer of protons during the desorption/ionization of analytes. The functionalized CdS NPs have desirable properties for the analysis of peptides in reflectron MALDI-TOF-MS with suppressed background noise and increased mass resolution (4-13-fold) in linear MALDI-TOF-MS. The application of CdS-MUA NPs and SA as the co-matrices in MALDI-MS is demonstrated for the analysis of hydrophobic proteins from soybean.     

Molecular weight determination of high molecular mass (glyco)proteins using CGE-on-a-chip, planar SDS-PAGE and MALDI-TOF-MS

The molecular weights (MW) of seven (glyco)proteins, of which five were plasma-derived, with MWs higher than 200 kDa were determined with three techniques: CGE-on-a-chip, SDS-PAGE and MALDI-TOF-MS. While the analysis of medium to high MW proteins with SDS-PAGE was an already well-established technique, the usefulness of MALDI-TOF-MS for the exact MW determination of high mass proteins was only partly described in literature so far. CGE-on-a-chip is the newest of all three applied techniques and was so far not applicable. Therefore, it was not evaluated for high MW (glyco)proteins. All proteins were analyzed under nonreducing as well as reducing conditions. In this work, it was demonstrated that all three described techniques were capable of determining the MW of all high molecular weight (glyco)proteins. The noncommercial CGE-on-a-chip assay allowed for the first time the electrophoretic separation of proteins in the MW range from 14 to 1000 kDa. MW assignment was limited to 500 kDa in the case of SDS-PAGE and 660 kDa in the case of the high MW CGE-on-a-chip assay. With the proper matrix and sample preparation, analysis with a standard MALDI-TOF-MS provided accurate MWs for all high MW proteins up to 1?MDa.