β-环糊精与1,2-苯并蒽络合的荧光研究

通过测量荧光寿命和荧光光谱,研究了1,2-苯并蒽(BA),9,10-二甲基-1,2-苯并蒽(DMBA)与β-环糊精(β-CD)络合过程及荧光猝灭。计算出络合平衡常数和猝灭常数。结果表明,BA与β-CD发生了络合作用,DMBA几乎不与β-CD络合。加入β-CD可使荧光分子的,聚集态与单体间的平衡向生成单体的方向移动,碘离子对BA的猝灭作用也明显减弱。

1,2,4-三氯苯胁迫对大豆下胚轴膜脂过氧化的影响

以盆栽法研究了不同浓度1,2,4-三氯苯(TCB)胁迫对大豆下胚轴膜脂过氧化作用的影响。结果表明,100—300μg·g-1TCB胁迫初期(1—3d)促使萌发大豆下胚轴内过氧化氢(H2O2)的积累显著增加,同时伴随质膜电解质渗漏率和组织自动氧化速率升高,显示发生膜脂质过氧化作用。TCB胁迫1—6d使活性氧清除酶功能紊乱,其中过氧化物酶(POD)活性升高,过氧化氢酶(CAT)活性开始上升后转为下降。推测大豆下胚轴受TCB胁迫伤害过程中,活性氧代谢失衡造成的膜脂质过氧化起着重要作用。

1,2,4-三氯苯胁迫对萌发大豆种子中活性氧的影响

以盆栽法研究了不同浓度 1,2 ,4 三氯苯 (TCB)胁迫对萌发大豆种子中活性氧代谢的影响 .结果表明 ,10 0～ 30 0 μg·g-1TCB胁迫初期 (1～ 3天 )促使萌发大豆种子呼吸强度升高及其峰值提前出现 ,超氧阴离子自由基 (O2 - )及过氧化氢 (H2 O2 )的积累显著增加 ,同时伴随丙二醛 (MDA)含量升高 ,显示发生膜脂质过氧化作用 .TCB胁迫 1～ 6天使活性氧清除酶功能紊乱 ,其中过氧化物酶 (POD)活性升高 ,超氧化物岐化酶 (SOD)活性开始上升后转为下降 .在萌发大豆种子受TCB胁迫伤害过程中 ,活性氧代谢失衡造成的膜脂质过氧化将起着重要作用 .

硬壳蛤性腺发育和卵母细胞成熟机理初步研究

采用体外药物诱导的方法，研究了5-羟色胺（5-hydroxytryptamine，5-HT）诱导的硬壳蛤卵母细胞成熟过程中cAMP信号通路的作用。结果表明，5-HT （0.01—100µM）均能够显著地诱导硬壳蛤卵母细胞的成熟。磷酸二酯酶抑制剂—咖啡因、茶碱和IBMX（3-异丁基-1-甲基黄嘌呤）可以单独抑制卵母细胞的自发成熟，但效果不显著。10mM的咖啡因和茶碱以及5mM的IBMX能够显著地抑制5-HT的诱导效果。dbcAMP（双丁酰基环腺苷一磷酸）不但能够抑制卵母细胞的自发成熟，而且还可以抑制5-HT诱导的成熟。因此，cAMP信号通路参与了5-HT诱导的硬壳蛤卵母细胞的成熟过程，并且该信号通路起着负调控的作用。 研究了PLC（磷脂酶C）和PKC（蛋白激酶C）的激活剂/抑制剂对5-羟色胺诱导的卵母细胞成熟的影响。高浓度的新霉素（PLC抑制剂）可以抑制5-HT诱导的卵母细胞的成熟，而DMBA（9,10-Dimethy-1,2-benzanthracene，9,10–二甲基胆蒽，PLC激活剂）则能够促进成熟。PMA（phorbol 12-myristate 13-acetate，佛波十四烷酸乙酸酯，PKC激活剂）能够抑制5-HT诱导的成熟，而Spingosine（PKC抑制剂）则可以促进卵母细胞的成熟。从而推测，5-HT诱导的卵母细胞成熟需要磷脂酰肌醇信号通路的激活。PLC浓度的降低能够抑制5-HT诱导的卵母细胞成熟；PKC浓度的降低则会促进卵母细胞的成熟。因此，在硬壳蛤卵母细胞的成熟过程中，PLC起促进的作用，DAG（二酰肌甘油）–PKC通路则起抑制的作用。 细胞外高浓度Ca2+能够促进硬壳蛤卵母细胞的成熟，Ca2+离子载体A23187也可以促进硬壳蛤卵母细胞的成熟。1-100µM异搏定（Verapamil，钙离子通道阻断剂）能够抑制卵母细胞的成熟，而100µM的Verapamil能够完全抑制其成熟。上述结果表明细胞外Ca2+对硬壳蛤卵母细胞的成熟是必需的，而且起到促进卵母细胞成熟的作用。三氟拉嗪（TFP，Ca2+与CaM结合的拮抗剂）能够抑制卵母细胞的成熟，高浓度的三氟拉嗪（1mM）能够完全抑制卵母细胞的成熟。说明CaM起到促进卵母细胞成熟的作用。可见，Ca2+通过与CaM的相互作用，共同起到促进硬壳蛤卵母细胞成熟的作用。 5-HT诱导成熟的卵母细胞可以完成受精过程，其受精过程以及幼虫发育情况与正常受精发育过程类似，没有显著差异。高浓度的新霉素可以抑制受精过程，而茶碱和咖啡因对受精没有影响。从而推测，磷脂酰肌醇信号通路参与了硬壳蛤卵母细胞的受精过程，而cAMP信号通路可能没有参与受精过程。 发现硬壳蛤的性腺发育与我国常见的双壳类如泥蚶相似。硬壳蛤卵母细胞中卵黄粒主要由线粒体、高尔基液泡、内质网和微吞饮泡形成。

Crystal structure of (5R,10R)-2,7-dibromo-3,8-dihydroxy-5,10-dimethoxy-5,10-dihydrochromeno[5,4,3-cde]chromene sesquihydrate, C16H12Br2O6 center dot 1.5H(2)O

C16H15Br2O7.5, orthorhombic, P2(1)2(1)2 (no. 18), a = 18.483(2) angstrom, b = 9.413(1) angstrom, c = 10.072(1) angstrom, V = 1752.3 angstrom(3), Z = 4, R-gt(F) = 0.083, wR(ref)(F-2) = 0.202, T= 293 K.

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。

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.

Mo掺杂对高纯Ce_(1-x)Nd_xO_(2-x/2)(x=0.10,0.15)体系烧结温度及晶界电性能的影响

用柠檬酸硝酸盐法制备高纯Ce1-xNdxO2-x/2(x=0.10,0.15)固溶体,加入摩尔分数为5%的Mo,研究了Mo掺杂对烧结温度、结构及电性能的影响.通过X射线衍射、电感偶合等离子体和场发射扫描电镜等手段对氧化物进行了结构表征,采用交流阻抗谱测试其电性能.柠檬酸硝酸盐法制备的前驱体经1450℃烧结24 h得到致密度大于96%的陶瓷材料;加入5%Mo,在1250℃下烧结8 h即可达到理想的致密度(>95%).加入Mo在烧结过程中可加快晶界迁移,促进晶粒生长,显著提高了晶界电导率.在600℃时Ce0.85Nd0.15O1.925的晶界电导率为2.56 S/m,加入Mo后材料的电导率增加到5.62 S/m.

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.

Development of a sensitive fluorescent derivatization reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC) and its application for determination of amino acids from seeds and bryophyte plants using high-performance liquid chromatography with fluorescence detection and identification with electrospray ionization mass spectrometry

A pre-column derivatization method for the sensitive determination of amino acids and peptides using the tagging reagent 1,2-benzo-3,4dihydrocarbazole-9-ethyl chloroformate (BCEOC) followed by high-performance liquid chromatography with fluorescence detection has been developed. Identification of derivatives was carried out by liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS/MS). The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent was replaced by 1,2-benzo-3,4-dihydrocarbazole functional group, which resulted in a sensitive fluorescence derivatizing reagent BCEOC. BCEOC can easily and quickly label peptides and amino acids. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography. The derivatives showed an intense protonated molecular ion corresponding m/z (M + H)(+) under electrospray ionization (ESI) positive-ion mode with an exception being Tyr detected at negative mode. The collision-induced dissociation of protonated molecular ion formed a product at m/z 246.2 corresponding to the cleavage of C-O bond of BCEOC molecule. Studies on derivatization demonstrate excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% are observed with a 3-4-fold molar reagent excess. Derivatives exhibit strong fluorescence and extracted detzvatization solution with n-hexane/ethyl acetate (10:1, v/v) allows for the direct injection with no significant interference from the major fluorescent reagent degradation by-products, such as 1,2-benzo-3,4-dihydrocarbazole-9-ethanol (BDC-OH) (a major by-product), mono- 1,2-benzo-3,4-dihydrocarbazole-9-ethyl carbonate (BCEOC-OH) and bis-(1,2-benzo-3,4-dihydrocarbazole-9-ethyl) carbonate (BCEOC)(2). In addition, the detection responses for BCEOC derivatives are compared to those obtained with previously synthesized 2-(9-carbazole)-ethyl chloroformate (CEOC) in our laboratory. The ratios AC(BCEOC)/AC(CEOC) = 2.05-6.51 for fluorescence responses are observed (here, AC is relative fluorescence response). Separation of the derivatized peptides and amino acids had been optimized on Hypersil BDS C-18 column. Detection limits were calculated from 1.0 pmol injection at a signal-to-noise ratio of 3, and were 6.3 (Lys)-177.6 (His) fmol. The mean interday accuracy ranged from 92 to 106% for fluorescence detection with mean %CV < 7.5. The mean interday precision for all standards was < 10% of the expected concentration. Excellent linear responses were observed with coefficients of > 0.9999. Good compositional data could be obtained from the analysis of derivatized protein hydrolysates containing as little as 50.5 ng of sample. Therefore, the facile BCEOC derivatization coupled with mass spectrometry allowed the development of a highly sensitive and specific method for the quantitative analysis of trace levels of amino acids and peptides from biological and natural environmental samples. (c) 2005 Elsevier B.V. All rights reserved.

Highly efficient and stable organic light-emitting diodes employing MoO3-doped perylene-3, 4, 9, 10-tetracarboxylic dianhydride as hole injection layer

We report highly efficient and stable organic light-emitting diodes (OLEDs) with MoO3-doped perylene-3, 4, 9, 10-tetracarboxylic dianhydride (PTCDA) as hole injection layer (HIL). A green OLED with structure of ITO/20 wt% MoO3: PTCDA/NPB/Alq(3)/LiF/Al shows a long lifetime of 1012 h at the initial luminance of 2000 cd/m(2), which is 1.3 times more stable than that of the device with MoO3 as HIL. The current efficiency of 4.7 cd/A and power efficiency of 3.7 lm/W at about 100 cd/m(2) have been obtained. The charge transfer complex between PTCDA and MoO3 plays a decisive role in improving the performance of OLEDs.

1.3-μm uncooled 10 Gb/s directly modulated MQW AlGaInAs/InP laser diodes

In this paper, we report a novel 1.3-μm uncooled AlGaInAs/InP multiple quantum well (MQW) ridge waveguide laser diodes. By optimizing the design of MQW structure and facet coatings, together with the application of reversed-mesa ridge waveguide (RM-RWG) structure, polyimide planarization, and lift-off processes technology, an uncooled 1.3-μm, 10-Gb/s directly modulated MQW ridge waveguide laser diode was successfully fabricated. The threshold current and the slope efficiency were 7 mA and 0.48 mW/mA, respectively. The directly modulated bandwidths of 11 and 9.2 GHz were achieved at room temperature and 80 Celsius degrees, respectively.

~(206)At的[лh_(1/2)vi_(13/2)~(-1)]10~-同质异能态研究(英文)

利用能量为６０－８０ＭｅＶ的~(１２)Ｃ束流，通过~１９７Ａｎ（~(１２)Ｃ，３ｎ）~２０６Ａｔ反应研究了~２０６Ａｔ核的高自旋能级结构．用７台ＢＧＯ（ＡＣ）ＨＰＧｅ探测器和一台用于探测低能γ射线的平面型ＨＰＧｅ探测器进行了γ射线的激发函数、γ－γ－ｔ符合及γ射线的角分布测量．基于这些测量，首次建立了包括２５条γ跃迁的~２０６Ａｔ高自旋能级纲图．确定了一个半寿命为（９０８±４００）ｎｓ、自旋和宇称为１０的同质异能态．基于较重的双奇核~(２０８，２１０ )Ａｔ能级结构的系统性，对~(２０６)Ａｔ的１０~－同质异能态进行了讨论．