MALDI-TOF-MS法用于谷脱甘肽S-转移酶分子量的测定

利用MALDI-TOF-MS法测定了谷胱甘肽S-转移酶的分子量,并讨论和对比了三种不同基质对其影响,认为用α-氰基-4-羟基肉桂酸(α-CHC)作基质是最佳适宜条件。实验结果表明本方法优于其它传统的测定生物大分子分子量方法。

Structure of [C8H7](+) and intramolecular proton transfer reactions in 3-phenyl-1-butyn-3-ol by MS/MS technique

The electron impact mass spectrum (EIMS) of 3-phenyl-1-butyn-3-ol was reported in this paper. Collision-induced dissociation (CID) was used to study the gas phase ion structure of [C8H7](+) formed by the fragmentation of ionized 3-phenyl-1-butyn-3-ol, and that it has the same structure as m/z 103 ions generated by cinnamic acid and alpha-methylstyrene. Deuterium labelling, metastable ion (MI) and CID experimental results indicate the formation of m/z 103 ion resulting from molecular ion of 3-phenyl-1-butyn-3-ol, which is a stepwise procedure via twice proton transfers, rather than concerted process during the successive elimination of methyl radical and neutral carbon monoxide accompanying hydrogen transfer. Moreover, in order to rationalized these fragmentation processes, the bimolecular proton bound complex between benzyne and acetylene intermediate has been proposed.

Studies on the product of ion-molecule reaction of halogeno-benzene in gas phase by MS/MS

The fragmentations of the product ions produced by the ion-molecule reaction of the halogeno-benzene (chlorobenzene, bromobenzene and iodobenzene) were studied using the collision-induced dissociation, The main product ions of the ion-molecule reaction of three kinds of halogeno-beneze include the dimeric ions, m/z(2M-X) ions and m/z(2M-2X) ions, The CID spectra of these ions were compared with that of the protonated bromodiphenyl and biphenyl, The formation mechanism and the structure of the product ions were obtained.

糖的基质辅助激光解吸/电离质谱(MALDI-MS)研究

通过糖类化合物３种常用基质ＭＡＬＤＩ－ＭＳ分析效果的比较以及寡糖和多糖正、负离子ＭＡＬＤＩ－ＭＳ谱的对比，找到了适合糖分析的基质２，５－ＤＨＢ，探讨了糖类化合物激光解吸／电离条件下形成离子的过程，指出了Ｎａ＋、Ｋ＋离子在寡糖分子量测定中的重要作用，借助柱层析分离手段，成功地测出了分子量大于１００００的葡聚糖的分子量．

酚醛环氧树脂的基质辅助激光解吸电离飞行时间质谱(MALDI-TOF-MS)表征

用基质辅助激光解吸电离飞行时间质谱（MALDI－TOF－MS）技术研究了F－46和JF－43型酚醛环氧树脂。获得了该类树脂的聚合度及其不同聚合度组分的分子结构；发现该类树脂中含有环氧氯丙烷的聚合物，给出了可能的分子结构。

5种E型环氧树脂的基质辅助激光解吸电离飞行时间质谱(MALDI-TOF-MS)表征

应用基质辅助激光解吸电离飞行时间质谱（ＭＡＬＤＩ－ＴＯＦ－ＭＳ）技术，研究了Ｅ－１２、Ｅ－３１、Ｅ－４２、Ｅ－４４和Ｅ－５１五种牌号环氧树脂。获得了该类树脂的聚合度及其不同聚合度所对应的分子结构；发现了该类树脂中有一定量的环氧氯丙烷的聚合物，并给出了可能的分子结构。

有机锡化合物的光电子能谱(XPS)和质谱(MS)研究Ⅱ

本文报道了７种新合成的（Ｚ）－１－［２－（三芳基锡）乙烯基］－１－环庚醇有机锡化合物的ＸＰＳ和ＭＳ结果。通过ＸＰＳ讨论了化合物中不同取代基的存在，对锡内层电子的影响及取代基对Ｏｌｓ结合能化学位移的作用。结果表明，卤素在这里起着重要的作用。通过ＭＳ和ＸＰＳ讨论了不同取代基对Ｏ→Ｓｎ键的影响。

单叶蔓荆子挥发油成分的GC/MS分析

采用气相色谱／质谱（ＧＣ／ＭＳ）联用技术对山东泰山产单叶蔓荆子挥发油的化学成分进行了分析，分离出３０多个峰，确认了其中２８种成分，占总离子流的９５％以上，并对挥发油的主要化学成分Δ３－蒈烯，用气相色谱／傅里叶红外光谱（ＧＣ／ＦＴＩＲ）法进行了验证。

金属富勒烯La＠C_（2n）的合成、提取及其ESR和MS表征

采用对掺入Ｌａ_２Ｏ_３的石墨棒原位活化并结合交换电极回放方法制备了产率较高的金属富勒烯，并用甲苯高温热提取的方法有效地提取出Ｌａ＠Ｃ_（２ｎ），其中Ｌａ＠Ｃ_（７４）为可溶性金属富勒烯增加了新成员．同时，首次采用解吸电子轰击质谱对提取物进行了表征，讨论了提取物的ＥＳＲ谱．

二甲基乙氧基乙烯基硅烷等离子体聚合物的的GC/MS研究

本文应用色谱—质谱(GS/MS)及裂解色谱质谱(Py/GC/MS)研究了二甲基乙氧基乙烯基硅烷(VDMES)等离子体聚合的气体冷凝物及聚合物膜。鉴别出多种化合物,并推导了等离子体聚合的反应历程,进而得到了气相反应与表面反应的实验依据。

CRYSTAL AND MOLECULAR STRUCTURES AND MS ANALYSE OF beta-CARBOXYLETHYL (OR alpha-METHYLETHYL) GERMANIUM TRICHLORIDES

This paper reports the results of the crystal and molecular structures, CI-MS and FAB-MS analyse of Cl3GeCH2CH2COOH and Cl3GeCH(CH3)CH2COOH. The characters and active parts of these molecules are also discussed

松花江水系有机污染的现状

本文介绍了GC、GC/MS、HPLC方法在分析松花江水系有机污染物中的应用。GC/MS、HPLC所用水样在现场处理,而TLC、GC样品在实验室处理。冬夏两次取样,共检出152种有机化合物,其中主要有机污染物55种,PAH_3占19％,氯化物占14％,芳烃占13％,其它占54％。

Product monitoring and quantitation of oligosaccharides composition in agar hydrolysates by precolumn labeling HPLC

Since the discovery of multiple bioactivities for agarobiose oligomers, a quantitative method has been in great need to monitor the agarobiose oligomers. This report demonstrates that agarobiose oligomers can be separated with high resolution in HPLC after introducing a-naphthylamine into compounds. Agarobiose oligomers ranged from biose to decaose were isolated by Sephadex column. HPLC analysis indicated that each oliomer could be quantified with good linearity and a low detection limit of 0.1-4 mug/ml. The chromatographic profiles of agaro-oligosaccharides with different hydrolysis modes (hydrochloride, citric acid, solid acid, and hydroxyl radical degradation) showed that agarobiose could be obtained more than 57.8% using solid acid mediated hydrolysis, while hydrochloride acid could degrade agar into a series of agaro-oligosaccharides from biose to decaose. The yield of oligosaccharides was low if hydrolyzed by citric acid. The Fenton degradation can increase the speed of hydrolysis, but the product was complex. (C) 2004 Elsevier B.V. All rights reserved.

Comparative analysis of astaxanthin and its esters in the mutant E1 of Haematococcus pluvialis and other green algae by HPLC with a C30 column

A gradient reversed-phase high-performance liquid chromatography (HPLC) method using a C30 column was developed for the simultaneous determination of astaxanthin, astaxanthin monoesters and astaxanthin diesters in the green algae Chlorococcum sp., Chlorella zofingiensis, Haematococcus pluvialis and the mutant E1, which was obtained from the mutagenesis of H. pluvialis by exposure to UV-irradiation and ethyl methanesulphonate (EMS) with subsequent screening using nicotine. The results showed that the contents of total astaxanthins including free astaxanthin and astaxanthin esters ranged from 1.4 to 30.9 mg/g dry biomass in these green algae. The lower total astaxanthin levels (< 2 mg/g dry biomass) were detected in the green algae Chlorococcum sp. and C. zofingiensis. The higher total astaxanthin levels (> 16 mg/g dry biomass) were found in the green alga H. pluvialis and its mutant E1. It is notable that the mutant E1 is found to have considerably higher amounts of total astaxanthin (30.9 mg/g) as compared to the wild strain of H. pluvialis (16.1 mg/g). This indicates that UV-irradiation and EMS compound mutagenesis with subsequent screening using nicotine is an effective method for breeding of a high-producing astaxanthin strain of H. pluvialis. In addition, the green alga C. zofingiensis had a remarkably higher percentage of astaxanthin diesters (76.3% of total astaxanthins) and a remarkably lower percentage of astaxanthin monoesters (18.0% of total astaxanthins) in comparison with H. pluvialis (35.5% for diesters and 60.9% for monoesters), the mutant E1 (49.1% and 48.1%) and Chlorococcum sp. (18.0% and 58.6%).

Determination of multiple trace elements in seawater using chelation ion chromatography and ICP-MS

An off-line chelation system combined with ICP-MS technique was developed for the quantitative determination of trace elements in seawater, namely V, Co, Ni, Cu, Zn, Mo, Cd, Pb, U and rare earth elements(REEs). The system was built based on an ion chromatography equipped with MetPac((R)) CC-I chelation columns which had a strong selective chelation to these target elements within a pH range 5.2-5.6. Acidified seawater samples and NH4Ac(2 mol/L) were blended to meet suitable pH before being injected into the chelation column, thus target elements were retained while alkali and alkaline metals were excluded. Then chelated elements were eluted by HNO3 (1 mol/L) and samples were collected for ICP-MS analysis. Varying the ratio of input( gen. 200 mL) to output( gen. 5 mL), the target elements which were concentrated as 40 times as their concentrations were far beyond instrumental quantification limits. At last, a certificated seawater CASS-4 was introduced and our detected values were in good agreement with those certified values.