pH-dependent assembly of 0D to 3D Keggin-based coordination polymers: Structures and catalytic properties

通讯作者地址: Long, LS (通讯作者), Xiamen Univ, State Key Lab Phys Chem Solid Surface, Xiamen 361005, Peoples R China 地址: 1. Xiamen Univ, State Key Lab Phys Chem Solid Surface, Xiamen 361005, Peoples R China 2. Xiamen Univ, Dept Chem, Coll Chem & Chem Engn, Xiamen 361005, Peoples R ChinaFour Keggin-based coordination polymers, namely, {[Cu-2(4,4'-bpy)(4,4'-Hbpy)(4)(H2O)(4)](-) (SiW12O40)(2)(H2O)(4)}(n) (1), {[Cu-2(4,4'-bpy)(4,4'-Hbpy)(6)(SiW12O40)(3)](4,4'-Hbpy)(2)(H2O)(7)}(n) (2), {[Cu-2(mu(2)-H2O)(2)(4,4'-bpy)(3)(SiW12O40)](H2O)(6)}(n) (3) and {[Cu-2(mu(2)-OH)(4,4'-bpy)(3)(SiW12O40)(H2O)] [Cu-2(mu(2)-O)(4,4'-bpy)(4)(H2O)(2)](0.5)center dot(H2O)(3)}(n) (4) (4,4'-bpy = 4,4'-bipyridine) were prepared through the hydrothermal reaction of silicotungstic acid, copper(II) nitrate and 4,4'-bipyridine under different pH conditions. Coordination polymers 1 and 2, which exhibit 0D and 1D structures respectively, were prepared at pH = 3.5. At pH = 5.5, a 2D coordination polymer 3 was obtained. Increasing the pH of the reaction to 8.5 led to a 3D coordination polymer 4. The structural diversities of 1-4 reveal that the pH value of the reaction plays a key role in the assembly of POM-based coordination polymers. Investigation of the catalytic properties of 1-4 for the oxidation of ethylbenzene indicates that the catalytic activity of the coordination polymers is closely related to the protonated extent of 4,4'-bpy in the coordination polymers.NNSFC 20825103 20721001 MSTC 2007CB815304 Fujian Province of China 2008J001

Calibration and Preliminary Application of Linear Quantitation Standard for Anti-HEV IgG Antibody

目的建立抗戊型肝炎病毒(Anti-HEV)IgG抗体的定量线性标准品,并进行初步应用。方法利用抗-HEV IgG和抗-HEV IgM ELISA检测试剂筛选出1份抗-HEV IgG阳性血清L9,经基因1型和4型的HEV ORF2C-端抗原及239抗原进行Western blot确认后,用WHO定量标准品,由3个实验室协作标定,利用量反应平行线法计算其抗-HEV IgG的含量。考察已标定的L9血清的稳定性,并用所标定的1.5倍系列稀释的血清对国内外6家抗-HEV IgG试剂的灵敏度进行检测。选择一灵敏度较高的试剂,在其线性范围内取L9的5个稀释度作为抗-HEV IgG抗体定量线性标准,对高、中、低浓度的3份临床血清重复检测5次,考察其重复性;对实验感染猴的系列血清中抗-HEV IgG含量进行定量检测,考核该定量线性标准品的应用效果;并对每次定量试验中的线性方程进行分析,确定相关系数r值和斜率k值的范围。结果经国内外试剂检测筛选出的阳性血清L9与基因1型和4型的HEV ORF2 C-端抗原及239抗原均有阳性反应。经协作标定,L9血清抗-HEV IgG含量为16.9U/ml。L9血清在-20℃下保存6、12、18个月,2～8℃保存24、48、96h后,定量结果均在95%置信区间内,且抗-HEV IgG含量均未明显下降。6家抗-HEVIgG检测试剂灵敏度差异较大,范围为0.03～5.00U/ml。确定L9血清从0.42U/ml开始的5个1.5倍系列稀释度,作为某一试剂抗-HEVIgG抗体定量线性标准品。利用该线性定量标准检测高、中、低浓度的3份临床血清,定量结果重复性较好;对实验感染猴系列血清进行定量检测,结果可有效地反映抗体水平变化趋势;94%的定量检测试验,r≥0.98,1.15≥k≥0.95。结论已建立了抗-HEVIgG抗体定量线性标准品,可用于疫苗免疫原性评价和流行病学调查。Objective To develop a linear quantitation standard for anti-hepatitis E virus (HEV) IgG antibody. Methods An anti-HEV IgG positive serum sample L9 was screened by using Anti-HEV IgM ELISA kit and Anti-HEV IgG ELISA kit and confirmed by Western blotting with HEV ORF2 C-terminal antigen of genotypes 1 and 4 and 239 antigen, then calibrated by 3 laboratories using WHO quantitation standard. Calculate the anti-HEV IgG content by dose-response parallel line assay, and evaluate the stability of calibrated serum sample. The sensitivities of 6 domestic and imported anti-HEV IgG ELISA kits were evaluated with the calibrated serum sample diluted 1. 5-fold serially. A linear quantitation standard for anti-HEV IgG antibody consisted of 5 dilutions of L9 within the linear determination range of a highly sensitive kit and evaluated for reproducibility by repeat test for 3 clinical serum samples, at high, moderate and low anti-HEV IgG contents respectively, for 5 times. The anti-HEV IgG contents in serum samples of HEV-infected monkeys were determined by the standard, and the determination curves were analyzed to define correlation coefficient r and slope k. Results Serum sample L9 showed positive reaction with HEV ORF2 C-terminal antigen of genotypes 1 and 4 and 239 antigen, and its anti-HEV IgG content was calibrated as 16. 9 U / ml. After storage at -20℃ for 6, 12 and 18 months or at 2 ～ 8℃ for 24, 48 and 96 h, all the quantitative determination results were within the 95% CI, and anti-HEV IgG content showed no significant decrease. The sensitivities of 6 kits evaluated with the L9 ranged from 0. 03 to 5. 00 U / ml. The linear quantitation standard for anti-HEV IgG antibody consisted of 5 dilutions of L9, starting from a concentration of 0. 42 U / ml. The determination results of 3 clinical serum samples showed good reproducibility of the standard. The determination results of sera of HEV-infected monkeys reflected the change of antibody level effectively. The r values of 94% of quantitative determination curves were not less than 0. 98, and the k values ranged from 1. 15 to 0. 95. Conclusion A linear quantitation standard for anti-HEV IgG antibody was established, which was suitable for the evaluation of immunogenicity and epidemical investigation of vaccine

大孔吸附树脂纯化芦笋皂苷工艺优化

以芦笋下脚料提取物作为原料,优化了大孔吸附树脂纯化芦笋皂苷的工艺。通过静态法,对8种大孔吸附树脂纯化芦笋皂苷的效果进行比较,结果表明HPD-100树脂纯化芦笋皂苷效果最佳,并对HPD-100大孔树脂纯化芦笋皂苷工艺进行了优化。在上样质量浓度15mg/mL、溶液处理量150mL、1mL/min流速过柱;吸附后,先用50mL蒸馏水洗去杂质,再用200mL80%乙醇洗脱,总皂苷的含量由14.26%提高到35.49%（mean±SD）。将初次纯化产物按照上述工艺再纯化一次,总皂苷含量可高于50%,达到国家五类新药的含量要求。HPD-100可较好地吸附分离芦笋皂苷,纯化效率高,且其操作简单、安全、成本低廉,有较高的推广应用价值

大孔吸附树脂纯化芦笋皂苷工艺优化

以芦笋下脚料提取物作为原料,优化了大孔吸附树脂纯化芦笋皂苷的工艺。通过静态法,对8种大孔吸附树脂纯化芦笋皂苷的效果进行比较,结果表明HPD-100树脂纯化芦笋皂苷效果最佳,并对HPD-100大孔树脂纯化芦笋皂苷工艺进行了优化。在上样质量浓度15mg/mL、溶液处理量150mL、1mL/min流速过柱;吸附后,先用50mL蒸馏水洗去杂质,再用200mL80%乙醇洗脱,总皂苷的含量由14.26%提高到35.49%（mean±SD）。将初次纯化产物按照上述工艺再纯化一次,总皂苷含量可高于50%,达到国家五类新药的含量要求。HPD-100可较好地吸附分离芦笋皂苷,纯化效率高,且其操作简单、安全、成本低廉,有较高的推广应用价值

芦笋叶绿素铜钠盐制备过程中提取工艺的研究

采用超声法对芦笋叶进行了叶绿素的提取并合成了叶绿素铜钠盐。结果表明,芦笋叶绿素的最佳提取工艺条件为：提取溶剂为80%丙酮与95%乙醇体积比1：4,提取时间60min,提取温度70℃,液固比10：1,超声功率160W。提取的叶绿素溶液,经过皂化、酸化、铜代、成盐等步骤制成叶绿素铜钠盐,得率（以鲜叶计）为0.18%,产品质量符合国家标准GB3262-1982

芦笋叶绿素铜钠盐制备过程中提取工艺的研究

采用超声法对芦笋叶进行了叶绿素的提取并合成了叶绿素铜钠盐。结果表明,芦笋叶绿素的最佳提取工艺条件为：提取溶剂为80%丙酮与95%乙醇体积比1：4,提取时间60min,提取温度70℃,液固比10：1,超声功率160W。提取的叶绿素溶液,经过皂化、酸化、铜代、成盐等步骤制成叶绿素铜钠盐,得率（以鲜叶计）为0.18%,产品质量符合国家标准GB3262-1982

芦笋叶绿素铜钠盐制备过程中提取工艺的研究

采用超声法对芦笋叶进行了叶绿素的提取并合成了叶绿素铜钠盐。结果表明,芦笋叶绿素的最佳提取工艺条件为:提取溶剂为80%丙酮与95%乙醇体积比1:4,提取时间60min,提取温度70℃,液固比10:1,超声功率160W。提取的叶绿素溶液,经过皂化、酸化、铜代、成盐等步骤制成叶绿素铜钠盐,得率(以鲜叶计)为0.18%,产品质量符合国家标准GB3262-1982

Filtration of the Cabbage Butterfly(Pieris rapae) N-Acetyl-β-D-Glucosaminidase Inhibitor

以菜青虫n-乙酰-β-d-氨基葡萄糖苷酶(nAgASE)为研究对象,比较了不同菜青虫部位来源及不同生长期的菜青虫nAgASE活性.结果表明,5龄虫和预蛹表皮来源的nAgASE比活最高.选取肉桂酸等天然化合物及其衍生物以及一些具有抗虫或杀虫活性的植物的粗提物,以其对菜青虫nAgASE的抑制作用为指标来粗筛nAgASE抑制剂.结果表明茴香酸、异丙基苯甲酸、间-羟基苯甲酸、2,4-二甲氧基苯甲酸以及肉桂酸对该酶具有一定的抑制效果,6 MMOl/l浓度可以分别使酶活力被抑制35.3%、25.9%、26.7%、29.1%和20.0%;银杏外种皮粗提物有较强的抑制效果,0.4 Mg/Ml的银杏酸可以让酶活力几乎完全丧失.上述结果提示有望从粗筛得到的几种植物中进一步分离纯化出高效的nAgASE抑制剂,为开发新型生物农药提供理论依据.We compared the specific activity of N-Acetyl-β-D-glucosaminidase(NAGase) from the larva of cabbage butterfly(Pieris rapae),the results showed that the specific activity of NAGase from the epidermis of cabbage butterfly larva was the highest among the specific activities of the NAGase from cabbage butterfly larva different parts,and the specific activity of NAGase from the five-age larva and pre-pupae are higher than other stages of the cabbage butterfly.Through the research on inhibitor effects of natural compounds and their derivants on NAGase activity and crude extract from plants on NAGase activity,the result indicated p-anisic acid,p-Isopropyl benzoic acid,m-Hydroxy benzoic acid,2,4-Dimethoxy benzoic acid and cinnamic acid,each 6 mmol/L,can obtain inhibit rate 35.3%,25.9%,26.7%,29.1% and 20.0%,respectively.And the effects of other compounds are far from satisfactory.The research on the inhibition effect of plants crude extract showed that crude extracts from the episperm of gingko billoba with water had strong inhibition effects.This research would serve as a theoretic basis for the development of bio-pesticide which had the major components of insect chitinolytic enzyme inhibitors.福建省自然科学基金(2006J0078);厦门大学细胞生物学与肿瘤细胞工程教育部重点实验室开放项目(2007102)资

太阳盐/钢渣定型复合相变储热材料的制备与性能研究

全球范围内的能源短缺和环境污染问题迫使人们积极开发可再生新能源。储热技术是解决新能源不稳定性问题的关键技术。相变材料是重要的储热介质之一。熔盐相变材料因其储热密度高,可操作温度范围广的优势,成为储热材料领域研究的热点。为解决熔盐液相易泄漏、低导热和高成本的问题,选择钢渣为基体材料,制备了太阳盐/钢渣定型复合相变储热材料,并通过扫描电子显微镜(SEM),热重–差示扫描量热法(TG–DSC),闪射法导热仪(LFA)和X射线衍射仪(XRD)对复合材料的微观结构、热性能和化学相容性进行了测试与表征。结果表明,钢渣与熔盐质量比5:5的复合材料定型效果最优。复合材料结构紧密;钢渣与熔盐化学相容性良好;复合材料潜热为64.0 kJ/kg,100～500℃内储热密度为945 kJ/kg,热导率高达2.23 W/(m·K)。太阳盐/钢渣复合相变储热材料不仅有利于储热技术的大规模应用,而且为钢铁工业废弃物回收利用提供了良好的参考,对节约资源、保护环境以及提高经济效益具有重要的意义

芦笋总皂苷的提取纯化及抗氧化研究

以芦笋总皂苷的提取率为考察指标,香草醛-冰醋酸法测定芦笋总皂苷的含量,采用正交设计法,对乙醇浓度、提取温度、提取时间、料液比4个因素进行考察,优化芦笋总皂苷提取工艺参数。芦笋总皂苷的最优工艺为:乙醇浓度为90%,提取温度为80℃,料液比为1∶40(g/mL),提取时间为1 h。在此条件下芦笋总皂苷提取率为10.68%。利用HPD-100大孔树脂对芦笋总皂苷提取液进行纯化,分别使用水、20%、50%、80%、95%的乙醇进行梯度洗脱。结果表明在乙醇浓度为50%的第3个流分时,总皂苷含量最高为51.0%。抗氧化试验表明,芦笋总皂苷纯化前后清除DPPH自由基的IC_(50)分别为147.43、140.05&mu;g/mL;清除ABTS+自由基的IC_(50)分别为212.76、169.70&mu;g/mL。</p