高效液相色谱/安培检测法测定蜂蜜中苯酚残留量

研究了用高效液相色谱 /安培检测法测定蜂蜜中苯酚残留量。考察了试验参数对测定结果的影响。在所选试验条件下 ,苯酚保留时间约为 12min ,检出限为 2 .0ng·g- 1。三组不同水平的加样回收率为 91.6 10 1.9% ,相对标准偏差 2 .812 .8%。测定结果满意     

大亚湾沉积物中氨基酸的垂直分布棗沉积物柱样W0中的游离氨基酸

用邻苯二甲醛（OPA）－3－巯基丙酸（3－MPA）柱前衍生高效液相色谱法测定了采自大亚湾近岸海域的一个长60cm的沉积物柱样W0中15种游离氨基酸（FAA）的含量，结果表明，W0中FAA总量在0．83－2．69mmol/kg之间，15种FAA以及FAA总量均随深度而以指数曲线降低，对氨基酸组成的分析表明，天冬氨酸，甘氨酸，组氨酸和苯丙氨酸的摩尔分数随深度而上升，苏氨酸，精氨酸，缬氨酸和异亮氨酸的摩尔分数随浓度而下降，其他氨基酸的摩尔分数随深度无显著变化，甘氨酸，丙氨酸，天冬氨酸，谷氨酸，丝氨酸是W0中含量最丰富的氨基酸，其摩尔数依次为28．1％，16．0％，14．7％，10．6％和7．2％。     

5-阿维菌素B1a酯的合成及生物活性

阿维菌素B_1a(AVB_1a)与羧酸在DMAP/DCC体系中直接酯化,得到10个5-AVB_1a酯衍生物,产率50%～79%;其化学结构由IR,¹H NMR,¹³CNMR和MS谱确证.生物活性测定结果表明,部分5-阿维菌素B_1a酯衍生物具有良好的杀虫、杀螨活性.     

聚丙烯熔融接枝马来酸酐反应机理的研究

改变聚丙烯（PP）熔融接枝马来酸酐（MAH）反应中的单体和引发剂的浓度以及添加适当助剂,考察了接枝产物的接枝率和恒定剪切应力（600kPa)及温度（210℃）下的剪切粘度,验证了作先前所提出的PP熔融接枝MAH的反应机理。即：在PP熔融接枝MAH的过程中,过氧化物自由基在熔融接枝过程中直接引发MAH单体及MAH单体在聚丙烯的大分子链段发生β断裂前直接被其引发而产生的接枝反应是影响产物的接枝率和分子量的关键。在不改变单体和引发剂浓度的情况下,降低过氧化物自由基在熔融接枝过程中直接引发MAH单体反应的程度而提高聚丙烯的大分子自由基直接引发MAH单体的反应趋势,是提高接枝产物接枝率和分子量的有效途径。     

Impact of Collection Volume and DNA Extraction Method on the Detection of Biomarkers and HPV DNA in First-Void Urine

The potential of first-void (FV) urine as a non-invasive liquid biopsy for detection of human papillomavirus (HPV) DNA and other biomarkers has been increasingly recognized over the past decade. In this study, we investigated whether the volume of this initial urine stream has an impact on the analytical performance of biomarkers. In parallel, we evaluated different DNA extraction protocols and introduced an internal control in the urine preservative. Twenty-five women, diagnosed with high-risk HPV, provided three home-collected FV urine samples using three FV urine collection devices (Colli-Pee) with collector tubes that differ in volume (4, 10, 20 mL). Each collector tube was prefilled with Urine Conservation Medium spiked with phocine herpesvirus 1 (PhHV-1) DNA as internal control. Five different DNA extraction protocols were compared, followed by PCR for GAPDH and PhHV-1 (qPCR), HPV DNA, and HBB (HPV-Risk Assay), and ACTB (methylation-specific qPCR). Results showed limited effects of collection volume on human and HPV DNA endpoints. In contrast, significant variations in yield for human endpoints were observed for different DNA extraction methods (p < 0.05). Additionally, the potential of PhHV-1 as internal control to monitor FV urine collection, storage, and processing was demonstrated.     

Controlling Metallophilic Interactions in Chiral Gold(I) Double Salts towards Excitation Wavelength‐Tunable Circularly Polarized Luminescence

Materials exhibiting excitation wavelength‐dependent photoluminescence (Ex‐De PL) in the visible region have potential applications in bioimaging, optoelectronics and anti‐counterfeiting. Two multifunctional, chiral [Au(NHC)₂][Au(CN)₂] (NHC=(4R,5R)/(4S,5S)‐1,3‐dimethyl‐4,5‐diphenyl‐4,5‐dihydro‐imidazolin‐2‐ylidene) complex double salts display Ex‐De circularly polarized luminescence (CPL) in doped polymer films and in ground powder. Emission maxima can be dynamically tuned from 440 to 530 nm by changing the excitation wavelength. The continuously tunable photoluminescence is proposed to originate from multiple emissive excited states as a result of the existence of varied Au^I???Au^I distances in ground state. The steric properties of the NHC ligand are crucial to the tuning of Au^I???Au^I distances. An anti‐counterfeiting application using these two salts is demonstrated.     

A Flexible Photoactive Titanium Metal–Organic Framework Based on a [TiIV3(μ3‐O)(O)2(COO)6] Cluster

The synthesis of titanium–carboxylate metal–organic frameworks (MOFs) is hampered by the high reactivity of the commonly employed alkoxide precursors. Herein, we present an innovative approach to titanium‐based MOFs by the use of titanocene dichloride to synthesize COK‐69, the first breathing Ti MOF, which is built up from trans‐1,4‐cyclohexanedicarboxylate linkers and an unprecedented [Ti^IV₃(μ₃‐O)(O)₂(COO)₆] cluster. The photoactive properties of COK‐69 were investigated in depth by proton‐coupled electron‐transfer experiments, which revealed that up to one Ti^IV center per cluster can be photoreduced to Ti^III while preserving the structural integrity of the framework. The electronic structure of COK‐69 was determined by molecular modeling, and a band gap of 3.77 eV was found.     

Mechanistic study of Ce-modified MnO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>/TiO<Subscript>2</Subscript> catalysts with high NH<Subscript>3</Subscript>-SCR performance and SO<Subscript>2</Subscript> resistance at low temperatures

A series of Ce–MnO _x /TiO₂ catalysts were prepared using a novel sol–gel template method and investigated for low-temperature selective catalytic reduction (SCR) of NO with NH₃ at temperatures ranging from 353 to 473 K. The 0.07Ce–MnO _x /TiO₂ catalyst showed the highest activity and best resistance to SO₂ poisoning. The structure and properties of the catalysts were characterized using X-ray diffraction (XRD) analysis, thermogravimetric analysis (TGA), thermogravimetry (TG)–differential scanning calorimetry (DSC)–mass spectroscopy (MS), high-resolution transmission electron microscopy (HRTEM), Brunauer–Emmett–Teller (BET) measurements, H₂-temperature-programmed reduction (TPR), and NH₃-temperature-programmed desorption (TPD). The superior catalytic activity of the 0.07Ce–MnO _x /TiO₂ catalyst was probably due to a change in the active components, an increase in surface active oxygen and surface acid sites, and lower crystallinity and larger surface area with Ce doping. Furthermore, the reduction ability also became stronger. The SO₂ poisoning resistance of the 0.07Ce–MnO _x /TiO₂ catalyst improved because doping with Ce can effectively decrease the formation of ammonium salt on the catalyst surface and the sulfation of MnO _x . In situ diffuse-reflectance infrared Fourier-transform (DRIFT) spectroscopy experiments indicated that addition of Ce could promote adsorption of NH₃ and inhibit generation of some nitryl species. The SCR reactions over the catalysts mainly followed the Eley–Rideal mechanism accompanied with a partial Langmuir–Hinshelwood mechanism.     

Fe掺杂Mn/TiO2低温脱硝催化剂的催化性能研究

采用氧化沉淀-浸渍法制备了不同含量Fe掺杂的Fe-Mn/TiO2低温脱硝催化剂,考察了催化剂在80~180 ℃范围内的脱硝能力并通过XRD、BET、TG、H2-TPR、NH3-TPD等测试手段,对催化剂的物理化学性质进行了表征.实验结果表明,Fe的加入并没有改变Mn/TiO2的主要晶相,仍是锐钛矿型的TiO2,MnOx和FeOx均以非晶态结构高度分散于载体表面,而且Fe的加入可以有效地改善催化剂的微观形貌、比表面积及表面酸性位点,从而提高其低温脱硝性能.Fe掺量在Fe/Ti为0.10时催化剂具有最佳性能,在120 ℃时脱硝率可达90;以上.