气相色谱-质谱法对鲜水果中5种保鲜剂残留量的同时测定

建立了气相色谱-质谱法(GC-MS)同时测定鲜水果中对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、乙萘酚、4-苯基苯酚和联苯醚5种保鲜剂的分析方法。鲜水果样品经乙醚超声提取、浓缩后,活性炭柱净化,选择离子模式(SIM)下测定,外标法定量。在优化条件下,5种保鲜剂的线性范围为0.2～4.0 mg/L,相关系数(r2)大于0.991,联苯醚的检出限为0.05 mg/kg,其余4种保鲜剂的检出限均为0.1 mg/kg。5种保鲜剂的加标回收率为80.4%～104.5%,相对标准偏差(RSD)为1.2%～6.4%。该方法简便、快速、试剂价廉易得,且能消除鲜水果样品中色素等杂质的干扰,具有较高的准确度和精密度,适用于鲜水果中上述5种防腐保鲜剂残留量的测定。     

澳洲茄胺单糖苷的合成及其抗肿瘤活性

以单糖为原料,经苯甲酰化保护和溴代制备中间体酰化溴代糖(3a～3e)。通过Koenigs-Knorr合成法将3a～3e与澳洲茄胺甙化缩合并脱保护合成了5个澳洲茄胺单糖苷化合物(5a～5e,5d和5e为新化合物),其结构经1H NMR,13C NMR和MS表征。用MTT法对5a～5e进行体外抗肿瘤细胞活性试验结果表明,5c和5d显示了较好的抗肿瘤活性。     

新型长链芳香酰胺聚合物的合成

3,5-二胺基苯甲酰胺与4,6-二烷氧基-1,3-苯二甲酰氯经缩合反应合成了两个新型的长链芳香酰胺聚合物,其结构经1H NMR,IR和GPC表征。     

Fe/MgO催化裂解甲烷制备碳纳米带

采用溶胶-凝胶法制备了Fe/MgO催化剂(E)。以甲烷为碳源,通过催化化学气相沉积法在E上生长出了碳纳米带(F),其结构和形貌经SEM和TEM表征。在最佳制备条件[E中Fe负载量为50%,甲烷流速70mL·min-1,于870℃反应1 h]下制备的F宽度约135 nm,厚约89 nm,长度在几十微米量级。     

Selective fluorescence response and magnetic separation probe for 2,4,6-trinitrotoluene based on iron oxide magnetic nanoparticles

Despite the rapid development of nanomaterials and nanotechnology, it is still desirable to develop novel nanoparticle-based techniques which are cost-effective, timesaving, and environment-friendly, and with ease of operation and procedural simplicity, for assay of target analytes. In the work discussed in this paper, the dye fluorescein isothiocyanate (FITC) was conjugated to 1,6-hexanediamine (HDA)-capped iron oxide magnetic nanoparticles (FITC–HDA Fe₃O₄ MNPs), and the product was characterized. HDA ligands on the surface of Fe₃O₄ MNPs can bind 2,4,6-trinitrotoluene (TNT) to form TNT anions by acid–base pairing interaction. Formation of TNT anions, and captured TNT substantially affect the emission of FITC on the surface of the Fe₃O₄ MNPs, resulting in quenching of the fluorescence at 519 nm. A novel FITC–HDA Fe₃O₄ MNPs-based probe featuring chemosensing and magnetic separation has therefore been constructed. i.e. FITC–HDA Fe₃O₄ MNPs had a highly selective fluorescence response and enabled magnetic separation of TNT from other nitroaromatic compounds by quenching of the emission of FITC and capture of TNT in aqueous solution. Very good linearity was observed for TNT concentrations in the range 0.05–1.5 μmol?L^?1, with a detection limit of 37.2 nmol?L^?1 and RSD of 4.7 % (n?=?7). Approximately 12 % of the total amount of TNT was captured. The proposed methods are well-suited to trace detection and capture of TNT in aqueous solution.

Hollow Multilayer Microcapsules for pH‐/Thermally Responsive Drug Delivery using Aliphatic Poly(urethane‐amine) as Smart Component

Hollow multilayer microcapsules made of aliphatic poly(urethane‐amine) (PUA) and sodium poly(styrene sulfonate) (PSS), templated on PSS‐doped CaCO₃ particles, are prepared for pH‐/thermally responsive drug delivery. The electrostatic interaction and hydrogen bonding under weak‐acid conditions between aliphatic PUA and PSS contribute to the formation of multilayer microcapsules. Scanning electron microscopy (SEM) results demonstrate an obvious variation of the hollow multilayer microcapsules in response to changes in temperature and pH value. Drug‐release behaviors using DOX as a model drug demonstrate that the drug release increases on decreasing the pH value because of the interaction weakness between aliphatic PUA and PSS in acidic conditions. Moreover, the drug release is higher at 55 °C than that at 37 °C for the sake of the shrinkage of aliphatic PUA above its lower critical solution temperature (LCST).

     

Separation,interconversion, and insecticidal activity of the cis‐ and trans‐isomers of novel hydrazone derivatives

A series of cis‐ and trans‐isomers of hydrazone derivatives were separated and analyzed through HPLC with diode‐array detection and HPLC‐MS/MS using ESI and ion trap MS. Two single crystals (A‐5‐1 and C‐2‐1) of the trans‐isomers were obtained and determined using X‐ray crystallography data, and the cis‐ to trans‐isomerization under different conditions was discussed. Both of the cis‐ and trans‐isomers of A‐4 and A‐5 exhibited good insecticidal activities against Plutella xylostella.     

Fast parallel detection of feline panleukopenia virus DNA by multi‐channel microchip electrophoresis with programmed step electric field strength

A multi‐channel microchip electrophoresis using a programmed step electric field strength (PSEFS) method was investigated for fast parallel detection of feline panleukopenia virus (FPV) DNA. An expanded laser beam, a 10× objective lens, and a charge‐coupled device camera were used to simultaneously detect the separations in three parallel channels using laser‐induced fluorescence detection. The parallel separations of a 100‐bp DNA ladder were demonstrated on the system using a sieving gel matrix of 0.5% poly(ethylene oxide) (M_r = 8 000 000) in the individual channels. In addition, the PSEFS method was also applied for faster DNA separation without loss of resolving power. A DNA size marker, FPV DNA sample, and a negative control were simultaneously analyzed with single‐run and one‐step detection. The FPV DNA was clearly distinguished within 30 s, which was more than 100 times faster than with conventional slab gel electrophoresis. The proposed multi‐channel microchip electrophoresis with PSEFS was demonstrated to be a simple and powerful diagnostic method to analyze multiple disease‐related DNA fragments in parallel with high speed, throughput, and accuracy.     

量子态选择的分子离子解离动力学：阈值光电子-光离子符合成像技术的应用

阈值光电子一光离子符合速度成像技术通过对光电子和符合的光离子同时进行速度聚焦控制,大幅提高了电子和离子的收集效率和离子平动能分辨率,成为开展气相分子光电离和光电离．解离动力学研究的有效工具．利用该技术,我们精确地测量了分子的电离能、离子出现势等重要参数,并且开展了若干具有量子态或内能选择的离子解离动力学研究,描绘了相关势能面存在浅势阱等重要动力学特征,讨论了不同振动态和电子态的激发对解离机理和产物通道的重要影响．