牛磺酸的稳定性及其在药酒中的测定

应用日立L-8800型全自动氨基酸分析仪测定了药酒中牛磺酸的含量及其稳定性。对仪器的分析条件作了两项调整,其一,梯度淋洗中淋洗剂B2的淋洗时间改为6.0 min;其二,自动进样器的进样模式改为“cut“模式。制备了3种浓度水平牛磺酸含量的药酒样品进行试验。每一试样又分为两份,一份在室温保存,另一份置于冰箱中在4℃保存。每份试样在制备的当时即按规定方法测定其牛磺酸含量,之后每隔1个月分析一次,连续测定3个月。测定结果证明,在药酒基体中,牛磺酸稳定性相当好。对同一试样分别进行5次测定,考核了方法的精密度,测得其RSD值为0.74%。测得此方法的回收率在97.3%至105.5%之间。     

冠醚化Schiff碱

综述了冠醚化Schiff碱的合成、配位和某些仿生性能的研究进展。     

某些西佛碱类化合物的质谱重排反应

研究了十四种西佛碱类化合物的电子轰击质谱，利用碰撞诱导解离(CID)和B/E联动扫描技术，证实了特殊重排产物的离子结构及生成机理，并利用亚稳离子测定方式对这类化合物的主要离子进行了归属。     

4-(3-吲哚基)-3-丁烯-2-酮苯甲酰腙Schiff碱过渡金属配合物的合成、表征及生物活性研究

A Schiff base ligand 4-[indol-3-yl]-but-3-en-2-one benzoyl hydrazone (HL), and its four transition metal complexes (ML₂，M=Cu(Ⅱ), Ni(Ⅱ), Zn(Ⅱ) and Co(Ⅱ)) have been prepared and characterized by means of elemental analysis, EI-MS, molar conductivity, IR, UV-Vis and ¹H NMR. The results showed that HL as a bidentate ligand coordinated with transition metal ions to form four-coordination complexes. The antibacterial activity was studied by using the filter scraps diffusion method, and the results indicated that the ligand and the complexes had a low bacteriostatic activity against S. Aureu, P. Aeruginosa and E. Coli. The low in vitro antitumor activity of the title complexes was also observed by using MTT method against KB, A2780, Bel7402 and HELF.     

噻吩甲酰基吡唑啉酮缩氨基酸稀土配合物的合成、表征及生物活性

A new amino-acid Schiff base, 1-phenyl-3-methyl-4-(2-thenoyl) pyrazolone-5-β-alanine (HL) and its ten rare earth complexes have been synthesized. On the basis of elemental analysis and molar conductance, the general formula of the complexes, [REL₂NO₃]·nH₂O (RE=La, Nd, Eu, Tb, Y, n=2; RE= Pr, Sm, n=1; RE= Dy, Er, Yb, n=3), is given. They were characterized by IR, UV-visible, ¹H NMR, ¹³C NMR and fluorescence. The results show that the rare earth ions exhibit coordination of eight in the complexes.The antibacterial experiments indicate that they have high antibacterial activities against S. Aureus, B. Subtillis, E. Coli, E. Carotovora and C. Flaccumfaciens.     

PMBP缩氨基酚的合成、晶体结构及抑菌活性

利用1－苯基－3－甲基－4－苯甲酰基－5－吡唑啉酮（PMBP）与邻、间、对氨 基酚合成了三种PMBP缩氨基酚Schiff碱，并进行了结构表征。PMBP缩邻氨基酚的X 射线衍射分析测定结果表明，该缩合反应是通过质子转移形式，形成了烯胺酮式结 构。抑菌活性测定结果表明它们对革兰氏阳性金黄色葡萄球菌和革兰氏阴性大肠杆 菌有较强的抑制作用。     

二聚体[Ni(TSSB)(Phen)(H2O)]·4H2O的合成、表征、晶体结构及热分解研究

The new compound, [Ni(TSSB)(Phen)(H₂O)]·4H₂O (TSSB=Taurine Salicylic Schiff Base, phen=O-Phenanthroline) has been synthesized and characterized by IR, elemental analysis and X-ray diffraction. The compound crystal data: triclinic, space group P1, a=1.049 7(2), b=1.122 5(2), c=2.384 3(4) nm, α=87.676(3)°, β=82.957(3)°, γ=62.924(3)°; V=2.482 3(7) nm³, Z=4; D_c=1.488 g·cm^-3, μ=0.920 mm^-1, F(000)=1 160, Goof=1.032, (Δρ)_max=899 e·nm^-3, (Δρ)_min=-624 e·nm^-3. The compound is a dimmer. In the complex, two Ni(Ⅱ) were coordinated by three oxygen atoms and three nitrogen atoms while the O atoms of Ac^- groups did not coordinate. The Ni(Ⅱ) formed a distorted octahedron geometry. The compound is an three dimensional net connecting with hydrogen bonding. CCDC: 275474.     

Co(II)Schiff碱配合物的合成、氧合反应热力学及热分解动力学的研究

合成了两种新的钴(II)schiff碱配合物水杨醛L-甲硫氨酸-水合钴(II)(1), 邻香兰素L-甲硫氨酸-水合钴(II)(2)。通过元素分析、红外光谱、热分析等测试手段研究了配合物的性质, 并确定了配合物的组成。用气体吸收装置测定配合物在乙腈溶液中不同温度下的饱和吸氧量, 求得氧合反应的平衡常数及热力学参数, 同时探讨了温度和配体结构对配合物氧合性能的影响。用TG-DTG法研究了配合物的热稳定性及非等温热分解动力学, 并采用积分法和微分法相结合的方法,推断了两种配合物的第一步热分解反应机理, 得到了热分解反应动力学参数及其动力学方程。     

介孔载体嫁接的Schiff碱铬配合物催化氧化苯甲醇合成苯甲醛

将Cr(salen)配合物分别嫁接于介孔SiO2,MCM-41和SBA-15上制备成非均相Schiff碱铬配合物,并用FT-IR,UV-Vis,XRD,N2吸附和元素分析等对非均相铬配合物进行了表征.以30%的H2O2为氧化剂,以非均相铬配合物为催化剂,在无有机溶剂、相转移催化剂和添加剂的条件下,研究了选择性催化氧化苯甲醇合成苯甲醛的反应.结果表明,非均相铬配合物都表现出较好的催化性能.选择不同的介孔载体对非均相铬配合物的催化性能有较大的影响,Cr(salen)/MCM-41配合物显示有最好的催化性能;在优化的反应条件下,苯甲醇转化率可达52.5%,苯甲醛选择性为100%,且该非均相铬配合物重复使用4次后仍保持较好的催化性能.