Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid‐phase dispersion extraction of bioactive flavonoids from toothpaste,plant, and saliva

This article describes the use of the mesoporous molecular sieve KIT‐6 as a sorbent in miniaturized matrix solid‐phase dispersion (MSPD) in combination with ultra‐performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT‐6 was used as a sorbent material for this mode of extraction. Compared with common silica‐based sorbents (C18 and activated silica gel), the proposed KIT‐6 dispersant with a three‐dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting “green chemistry” requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02–0.04 μg/mL and 0.07–0.13 μg/mL, respectively. Finally, the miniaturized matrix solid‐phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained.     

新型核素~(64)Cu标记硝基咪唑类肿瘤乏氧显像剂及正电子发射断层扫描显像研究

采用新型核素64Cu标记了含丙烯胺肟[Pn AO(3,3,9,9-Tetramethyl-4,8-diazaundecane-2,10-dione Dioxime)]结构的硝基咪唑类乏氧显像剂Pn AO-1-(2-nitroimidazole)[BMS181321],通过优化反应条件,于室温下反应10 min后即得到高放化纯度和高比活度的标记化合物64Cu-BMS181321.目标产物经放射性高效液相色谱检测验证和体外稳定性实验确认后,通过尾静脉注射到人源胰腺癌(PANC-1细胞系)裸鼠体内,分别于注射显像剂4和8 h后进行小动物正电子发射断层扫描显像(Micro-PET).结果表明,4 h左右肿瘤乏氧区域有良好的放射性浓聚.64Cu-BMS181321的合成及其分子显像研究开创了64Cu标记硝基咪唑类乏氧显像剂进行乏氧显像的先例,经进一步药物临床实验评价后,64Cu-BMS181321有望成为具有良好前景的PET乏氧显像药物.     

自交联共轭亚油酸囊泡的温敏膨胀行为

采用紫外辐照引发共轭亚油酸(CLA)囊泡内聚合反应,获得自交联CLA囊泡.用动态激光光散射(DLS)和冷冻透射电子显微镜(cryo-TEM)等观察自交联CLA囊泡的粒径和形貌变化,结果表明,自交联CLA囊泡的囊泡结构不仅不随温度变化解体,而且表现出明显的温敏膨胀性.自交联CLA囊泡体外释放5-氟尿嘧啶的实验表明其具有温度响应的缓释和控释特性.     

吡喃盐化合物的合成及应用研究进展

吡喃盐是一类具有独特化学反应活性和光物理性质的杂环化合物,在有机合成、生物传感和光电材料等许多领域展现了良好的应用前景.结合本课题组的研究成果,综述了α-非活性吡喃盐和α-活性吡喃盐化合物的合成研究进展,并介绍了一些典型吡喃盐化合物在有机合成、光敏剂、离子液体和荧光传感材料等领域的应用.     

微管蛋白聚合抑制剂OXi8006的合成新方法

2-(3'-羟基-4'-甲氧基苯基)-3-(3",4",5"-三甲氧基苯甲酰基)-6-甲氧基吲哚(OXi8006)能够有效抑制微管蛋白聚合,而表现出良好抗癌活性.目前报道的OXi8006全合成路线较长、总收率低,且反应条件苛刻.为了更高效地合成该化合物,从而为进一步的活性和构效关系研究提供原料.以廉价易得的异香兰素为起始原料,先合成芳基乙炔,再与3,4,5-三甲氧基苯甲醛通过亲核加成、氧化反应获得二芳基炔酮、二芳基炔酮再与邻碘代苯胺通过杂迈克尔加成和分子内Heck反应构建出OXi8006的主体结构——2-芳基-3-芳酰基取代吲哚,从而缩短了合成路线,并使总收率提高到20%.     

Simple and Sensitive Voltammetric Determination of Esculetin Using Electrochemically Reduced Graphene Oxide Modified Electrode

A simple and sensitive voltammetric sensor for esculetin, based on electrochemically reduced graphene oxide film modified glassy carbon electrode, was reported for the quantitative determination of esculetin in the Chinese traditional herbal drug Viola yedoensis Makino. Electrochemical impedance spectroscopy and scanning electron microscopy were employed to study the characteristic of the graphene oxide film. The electrochemical behavior of esculetin on this sensor was investigated in pH 3.0 phosphate buffer solution by cyclic voltammetry. Significant advantages were achieved by the excellent conductivity and the high surface‐to‐volume ratio of electrochemically reduced graphene oxide. A calibration plot of oxidation peak currents versus esculetin concentrations was linear in the range of 4.0 ξ 10^‐8 mol L^‐1 to 5.0 ξ 10^‐6 mol L^‐1 with a detection limit of 2.0 ξ 10^‐8 mol L^‐1. The practical application of the present sensor was demonstrated by determining the concentration of esculetin in real sample with no interference.     

New Monoterpenoids from Fruits of Gardenia jasminoides var. radicans

One new lactone, cyclopentanepyrone A ( 1 ), and two new monoterpenoids, gardeterpenone A ( 2 ) and jasminoside V ( 3 ), were isolated from the fruits of Gardenia jasminoides var. radicans, along with four known monoterpenoids, 4 – 7 , which were isolated from this plant for the first time. The structures of the isolates were elucidated by extensive spectroscopic studies, including UV, IR, 1D‐ and 2D‐NMR, ESI‐MS, HR‐ESI‐MS, and CD experiments.