Ce_(0.9)RE_(0.1)P_5O_(14)晶体中Ce~(3+)的发光寿命研究

利用时间相关单光子计数方法系统地测定了Ce_(0.9)RE_(0.1)P_5O_(14)晶体中Ce~(3+)的发光寿命。发现荧光寿命数值能够较好地说明双掺晶体中除Ce而外的其它稀土离子对Ce~(3+)的发光强度的增强或猝灭现象。

1,5,9-环十二碳三烯的阳离子型跨环齐聚合反应

本文研究1,5,9-环十二碳三烯在阳离子型引发剂AlCl_3和BF_3·OEt_2催化下进行的跨环聚合反应,考察各种反应条件对跨环聚合反应的影响。产物为白色粉末,分子量均在1096—1431之间。对其溶解性、核磁共振和红外光谱的分析,确认了它的结构。

Ce_(0.9)Yb_(0.1)P_5O_(14)晶体的光电压光谱

前文在研究五磷酸铈晶体中Ln~(3+)对Ce~(3+)发光强度的影响时,发现当加入少量的Eu~(3+)和Yb~(3+)离子到CeP_5O_(14)晶体中能使Ce~(3+)的发射产生严重的猝灭现象,以致于用Ce~(3+)的302nm吸收带激发晶体时,观察不到Ce~(3+)的发射,或者十分微弱。令人费解的是Yb~(3+)离子在紫外和可见区无吸收带,Yb~(3+)离子的加入应该成为一个稀释离子,现却使Ce~(3+)的发射产生严

New sphingolipids with a previously unreported 9-Methyl-C-20-sphingosine moiety from a marine algous endophytic fungus Aspergillus niger EN-13

Asperamides A (1) and B (2), a sphingolipid and their corresponding glycosphingolipid possessing a hitherto unreported 9-methyl-C-20-sphingosine moiety, were characterized from the culture extract of Aspergillus niger EN-13, an endophytic fungus isolated from marine brown alga Colpomenia sinuosa. The structures were elucidated by spectroscopic and chemical methods as (2S,2'R,3R,3'E,4E,8E)-N-(2'-hydroxy-3'-hexadecenoyl)-9-methyl-4,8-icosadien-1,3-diol (1) and 1-O-beta-D-glucopyranosyl-(2S,2'R,3R,3'E,4E,8E)-N-(2'-hydroxy-3'-hexadecenoyl)-9-methyl-4,8-icosadien-1,3-diol (2). In the antifungal assay, asperamide A (1) displayed moderate activity against Candida albicans.

青海歧穗大黄及其生长土壤中9种无机元素含量特征

为对比青海高原境内不同生境歧穗大黄中9种无机元素含量特征,用原子吸收光谱法分析了其宏量元素K、Na、Ca、Mg、P及微量元素Cu、Zn、Fe、Mn含量.结果表明,青海歧穗大黄植物与其土壤环境呈现出不同的无机元素含量特征,但一致表现为Ca和P在植物的富集,且植物中P含量随海拔升高而明显增加,Zn含量随海拔升高而增加.

荧光衍生试剂1-[2-（对甲苯磺酸醋）乙基]2-苯基咪唑[4,5-f]9,10-菲的合成及其在长链脂肪酸分析中的应用

合成了新的荧光衍生试剂1-[2-（对甲苯磺酸酯）乙基]-2-苯基咪唑[4,5-f]9,10-菲（TsEPIP），并将其作为柱前衍生化试剂，在Eclipse XDB-C：色谱柱上采用梯度洗脱实现了11种长链（C_(20)～C_(30)）游离脂肪酸（FFA）衍生物的基线分离。利用柱后在线的串联质谱并以大气压化学电离源（APCI）的正离子模式实现了各组分的质谱定性。对土壤及3种苔醉（东亚毛灰鲜、锦丝鲜、羽平鲜）中FFA组分的定量结果表明，苔鲜植物从土壤中富集了大量的长链游离脂肪酸。荧光检测的激发波长和发射波长分别为260 nm和380 nm。线性回归系数大于0.9996，检测限为26.19～76.67 fmol。所建立的方法具有良好的重现性，对实际样品的测定结果令人满意。

9种“藏茵陈”原植物中的7种有效化学成分研究

目的 研究藏药市场上9种“藏茵陈”植物中有效化学成分，根据所含成分的差异及其生理活性，确定这些植物的药用价值。方法 采用HPLC法测定7种成分的量。结果 9种植物的有效成分差异很大。结论 针对不同的化学成分用途，选择不同的植物，有效利用资源。[著者文摘]

青海青甘韭9个居群的核型

本文研究了青海葱属青甘韭 9个居群的染色体数目和核型。其中分布于湟源、西宁和共和海拔相对较低的地区的居群为 2倍体 ,核型公式为 2n =2x =16 =14m +2st (2SAT) (湟源居群和西宁居群 ) ,2n =2x =16 =12m +2sm +2st (2SAT) (共和居群 ) ;分布于玛沁、玉树、囊谦等高海拔地区的居群为 4倍体 ,核型公式为 2n =4x =32 =2 8m +4st (2SAT) (玉树居群 1和囊谦居群 1) ,2n =4x =32 =2 4m +4sm +4st (玛沁居群和玉树居群 3)和 2n =4x =32 =2 6m +2sm+4st (玉树居群 2 ) ;囊谦一个生长在林下的居群为8倍体，2n =8x =64 =54m +2sm +8st.讨论了居群间的核型分化和倍性与分布的关系。

CE determination of 2-(9-carbazole)ethyl chloroformate-labeled oligopeptides

A pre-column derivatization method for sensitive determination of oligopeptides, using the tagging reagent 2-(9-carbazole)ethyl chloroformate (CEOC-Cl) followed by capillary electrophoresis (CE) with diode-array detection, has been developed. Maximum yield close to 100% were observed when a three to fourfold molar excess of reagent was used at pH 9.0-10.0. Excess reagent was extracted with n-hexane-ethyl acetate 9:1-10:1 (v/v); this enabled direct analysis using CE with no significant disturbance from the major fluorescent reagent degradation by-products. The effects on the results of buffer pH and of SDS and organic modifier concentrations were examined. Good baseline resolution in the separation of five CEOC-peptides was achieved with a 48.5-cm total length (effective length 40 cm) 50-mu m inner diameter capillary column.

Pre-column derivatization of amines with 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate followed by LC-fluorescence and LC-APCI-MS

A pre-column derivatization method for the sensitive determination of amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate (BCIC-Cl) followed by high-performance liquid chromatography with fluorescence detection has been developed. Identification of derivatives is carried out by high performance liquid chromatography/atmospheric pressure chemical ionization (LC-APCl-MS-MS). The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent is replaced by 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl functional group, which results in a sensitive fluorescence derivatizing reagent BCIC-Cl. BCIC-Cl can easily and quickly label amines. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography and show an intense protonated molecular ion corresponding m/z [MH](+) under APCl in positive-ion mode. The collision-induced dissociation of protonated molecular ion formed a product at m/z 260 corresponding to the cleavage of CH2-OCO bond. Studies on derivatization demonstrate excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% are observed with a 3 to 4-fold molar reagent excess. In addition, the detection responses for BCIC derivatives are compared with those obtained using CEOC and FMOC as derivatization reagents. The ratios of l(BCIC)/l(CEOC) and l(BCIC)/l(FMOC) are, respectively, 1.23-3.14 and 1.25-3.08 for fluorescent (FL) responses (here, l is relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C-8 column. Detection limits are calculated from 1.0 pmol injection, at a signal-to-noise ratio of 3, are 10.6-37.8 fmol. The mean interday accuracy ranges from 94 to 105% for fluorescence detection with the largest mean %CV < 7.5. The mean interday precision for all standards is < 6.0% of the expected concentration. Excellent linear responses are observed with coefficients of > 0.9997.

2-(2-Phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA) and its application for determination of amines by high performance liquid chromatography with fluorescence detection and identification with mass spectroscopy/atmospheric pressure chemical ionization

A simple, sensitive, and mild method for the determination of amino compounds based on a condensation reaction with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC-HCI) as the dehydrant with fluorescence detection has been developed. Amines were derivatized to their acidamides with labeling reagent 2-(2-phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA). Studies on derivatization conditions indicated that the coupling reaction proceeded rapidly and smoothly in the presence of a base catalyst in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maximum at lambda(ex) 260nm and an emission maximum at lambda(em) 380nm. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by high-performance liquid chromatography. Identification of derivatives was carried out by online post-column mass spectrometry (LC/APCI-MS/MS) and showed an intense protonated molecular ion corresponding m/z [MH](+) under APCI in positive-ion mode. At the same time, the fluorescence properties of derivatives in various solvents or at different temperature were investigated. The method, in conjunction with a gradient elution, offered a baseline resolution of the common amine derivatives on a reversed-phase Eclipse XDB-C-8 column. LC separation for the derivatized amines showed good reproducibility with acetonitrile-water as mobile phase. Detection limits calculated from 0.78 pmol injection, at a signal-to-noise ratio of 3, were 3.1-18.2 fmol. The mean intra- and inter-assay precision for all amine levels were < 3.85% and 2.11%, respectively. Excellent linear responses were observed with coefficients of > 0.9996. The established method for the determination of aliphatic amines from real wastewater and biological samples was satisfactory. (c) 2006 Elsevier B.V. All rights reserved.