微生物法分析天然抗氧化剂性能

建立了微生物抑菌活性纸片试验法，对葛根黄酮、诃子提取物、丹皮酚、竹叶黄酮等4种天然抗氧化剂的抗氧化性能进行了研究。竹叶黄酮、诃子、葛根具有较强的抗单线态氧能力，而丹皮酚抗单线态氧的能力较差。在不同的氧化还原微环境下，天然抗氧化剂可能表现出抗氧化能力，亦可能表现出促氧化能力，二者有着不同的反应机理。微生物抑菌活性纸片法可作为研究较复杂生物环境中抗氧化剂性能的一种简便方法。     

取代肉桂酰甘氨酸酯的合成

在N-甲基吡咯烷酮(NMP)促进下,取代肉桂酸(1a^1g)与二氯亚砜(SOCl2)在20℃酰氯化反应0.5 h,再加入甘氨酸乙酯盐酸盐,在40℃下酰胺化反应4 h,n(取代肉桂酸)/n(SOCl2)/n(甘氨酸乙酯盐酸盐)=1.0/1.2/1.4,合成了一系列取代肉桂酰甘氨酸乙酯(2a^2g),其结构经1H NMR、13C NMR、IR和MS(EI)确证。并探讨了NMP促进取代肉桂酰甘氨酸乙酯反应可能的机理。     

用FTIR定量测定聚对苯二甲酸乙二酯晶区和非晶区反式构象含量

用傅里叶变换红外分光光度计测定不同条件下退火处理的聚对苯二甲酸乙二酯膜的谱图, 用谱带分离技术对归属于反式构象的1340cm^-^1谱带进行阻尼最小两乘分峰处理, 结合属左右式构象贡献的1454cm^-^1谱带, 用线性回归分析的方法获得晶区反式构象、非晶区反式构象、非晶区左右式构象的百分含量。     

微波辅助快速制备2D/1D ZnIn2S4/TiO2 S型异质结及其光催化制氢性能

The threat and global concern of energy crises have significantly increased over the last two decades. Because solar light and water are abundant on earth, photocatalytic hydrogen evolution through water splitting has been considered as a promising route to produce green energy. Therefore, semiconductor photocatalysts play a key role in transforming sunlight and water to hydrogen energy. To date, various photocatalysts have been studied. Among them, TiO₂ has been extensively investigated because of its non-toxicity, high chemical stability, controllable morphology, and high photocatalytic activity. In particular, 1D TiO₂ nanofibers (NFs) have attracted increasing attention as effective photocatalysts because of their unique 1D electron transfer pathway, high adsorption capacity, and high photoinduced electron–hole pair transfer capability. However, TiO₂ NFs are considered as an inefficient photocatalyst for the hydrogen evolution reaction (HER) because of their disadvantages such as a large band gap (~3.2 eV) and fast recombination of photoinduced electron–hole pairs. Therefore, the development of a high-performance TiO₂ NF photocatalyst is required for efficient solar light conversion. In recent years, several strategies have been explored to improve the photocatalytic activity of TiO₂ NFs, including coupling with narrow-bandgap semiconductors (such as ZnIn₂S₄). Recently, microwave (MW)-assisted synthesis has been considered as an important strategy for the preparation of photocatalyst semiconductors because of its low cost, environment-friendliness, simplicity, and high reaction rate. Herein, to overcome the above-mentioned limiting properties of TiO₂ NFs, we report a 2D/1D ZnIn₂S₄/TiO₂ S-scheme heterojunction synthesized through a microwave (MW)-assisted process. Herein, the 2D/1D ZnIn₂S₄/TiO₂ S-scheme heterojunction was constructed rapidly by using in situ 2D ZnIn₂S₄nanosheets decorated on 1D TiO₂ NFs. The loading of ZnIn₂S₄ nanoplates on the TiO₂ NFs could be easily controlled by adjusting the molar ratios of ZnIn₂S₄ precursors to TiO₂ NFs. The photocatalytic activity of the as-prepared samples for water splitting under simulated solar light irradiation was assessed. The experimental results showed that the photocatalytic performance of the ZnIn₂S₄/TiO₂ composites was significantly improved, and the obtained ZnIn₂S₄/TiO₂ composites showed increased optical absorption. Under optimal conditions, the highest HER rate of the ZT-0.5 (molar ratio of ZnIn₂S₄/TiO₂= 0.5) sample was 8774 μmol·g^-1·h^-1, which is considerably higher than those of pure TiO₂ NFs (3312 μmol·g^-1·h^-1) and ZnIn₂S₄nanoplates (3114 μmol·g^-1·h^-1) by factors of 2.7 and 2.8, respectively. Based on the experimental data and Mott-Schottky analysis, a possible mechanism for the formation of the S-scheme heterojunction between ZnIn₂S₄ and TiO₂ was proposed to interpret the enhanced HER activity of the ZnIn₂S₄/TiO₂heterojunctionphotocatalysts.      

火焰和石墨炉原子吸收光谱法对大米中金属元素含量的测定分析

采用火焰和石墨炉原子吸收光谱法对随机抽取的江西省、吉林省共五种大米中的Fe、Cu、Zn、Mn、Ca、Pb等六种金属元素进行了测定。结果表明,江西省大米中的金属元素含量均略高于吉林省前谷县达里巴乡大米,这可能与南北土壤中金属元素的分布不同有关。     

2-[2-(4, 6-二甲基)-嘧啶基]-4-苯基-1, 2, 4-恶二唑烷-3, 5-二酮的合成

异氰酸苯酯和N-[2-(4, 6-二甲基)-嘧啶基]-羟胺(5)反应生成1-[2-(4, 6-二甲基)-嘧啶基]-1-羟基-3-苯基脲(6)。化合物(6)在三乙胺存在下和氯甲酸乙酯反应生成2-[2-(4, 6-二甲基)-嘧啶基]-4-苯基-1, 2, 4-恶二唑烷-3, 5-二酮(1)。     

溶胶-凝胶法制备还原态K-Co-Mo催化剂的合成醇性能

应用溶胶-凝胶法制备了还原态K-Co-Mo催化剂, 比较了不同的组分和不同的反应条件对合成醇性能的影响。实验结果表明，适量钾和钴助剂的添加能显著提高催化剂合成醇的性能，尤其是提高了C2+醇的选择性。此外，反应温度、压力以及空速对合成醇影响明显，升高温度可以提高催化反应中低碳醇的收率，但选择性下降；增加压力和空速可以提高低碳醇的收率和选择性，对合成低碳醇有利。在230 ℃，6.0 MPa，14 400 h－1条件下，催化剂合成低碳醇的收率为375.4 g/kg·h，选择性为70.2%，C1OH/C2+OH为0.48。     

表面活性剂增敏2.5次微分极谱测定香豆素

拟定了表面活性剂增敏、2 .5次微分极谱测定香豆素的方法。在含 6.0× 10 -6 mol·L-13 氯 2 羟丙基 三甲基氯化铵的 0 .1mol·L-1KH2 PO4 Na2 HPO4 (pH 6.8)缓冲液中 ,香豆素还原波 [峰电位Ep=- 1.60V(vs .SCE) ]的 2 .5次微分极谱峰峰电流e″p 与其浓度在 4 .0× 10 -7～ 6.0× 10 -5mol·L-1范围内呈良好线性关系 (r =0 .9998,n =10 ) ,检出限为 1.2× 10 -7mol·L-1。 13次平行测量 8.0× 10 -6 mol·L-1香豆素的峰电流 ,RSD为 1.5 %。该方法可用于中药白芷中香豆素的直接测定     

毛细管区带电泳法测定复方甘草片中的甘草酸、甘草次酸、吗啡和苯甲酸钠

 在紫外检测波长为 2 2 8nm、电压为 14kV、背景电解质为 5 0mmol/L硼砂溶液、内标为氢氯噻嗪的条件下 ,用毛细管区带电泳法对复方甘草片中的甘草酸、甘草次酸、吗啡和苯甲酸钠进行了定量分析。结果甘草酸、甘草次酸、吗啡和苯甲酸钠的相对峰面积 (组分与内标的峰面积之比 )与各自的质量浓度之间呈良好的线性关系 ,上述 4种组分的平均回收率分别为 98 2 % ,97 3% ,97 1%和 97 5 %。方法简便、快速、准确。     

锡—邻菲咯啉络合物吸附极谱波的研究及应用

研究了锡－邻菲咯啉体系的极谱行为，在ｐＨ＝２．５０的０．１０ｍｏｌ／Ｌ氯乙酸－氯乙酸钠介质中，在单扫描极谱上，Ｓｎ－邻菲咯啉络合物于－０．４１Ｖ电位处产生一良好的吸附还原波。波高与Ｓｎ的浓度在２．０×１０＾－８－４．０×１０＾－６ｍｏｌ／Ｌ范围内呈线性关系；检出限为１．０×１０＾－８ｍｏｌ／Ｌ Ｓｎ，对合金标样中的锡进行测定，取得了满意的结果。