固相萃取-液相色谱-串联质谱法检测小鼠肌肉组织中矮壮素

建立了快速检测小鼠肌肉组织中矮壮素的固相萃取-液相色谱-串联质谱(SPE-LC-MS/MS)方法。小鼠肌肉样品经乙腈提取,弱阳离子交换(WCX)固相萃取柱净化,3 mL甲酸-甲醇(1∶99,V/V)重力洗脱。采用亲水作用色谱柱(HILIC),含10 mmol/L乙酸铵、0.1%甲酸水溶液-乙腈(40∶60,V/V)为流动相,以电喷雾正离子(ESI+)、多反应监测模式(MRM)进行矮壮素的定性分析,采用基质标准曲线外标法进行定量分析。结果表明:矮壮素的线性范围为5.0～500.0μg/L,线性相关系数为0.9991。在10.0,100.0和200.0μg/kg添加浓度下的回收率为73.2%～82.3%;相对标准偏差小于9.3%;方法定量限为10.0μg/kg,能够满足小鼠肌肉组织中痕量矮壮素检测的要求。     

含反式环己烷结构的C-葡萄糖苷类SGLT2抑制剂的合成及其降血糖活性Ⅱ

设计并合成了一系列新型含反式-4-烷基环己烷结构的C-葡萄糖苷类SGLT2抑制剂——反式-1-{4-甲氧基-3-[(4-取代环己基)甲基]苯基}-1-脱氧-β-D-吡喃葡萄糖(12a～12d),其结构经1H NMR和MS表征.小鼠口服糖耐量实验表明,12a～12d均显示较强的降血糖活性.对12a～12d进行了较为完整的构效关系分析,得到了良好的构效关系.     

新型含偕二甲基结构的PAR-1拮抗剂的合成及其抗血小板聚集活性

以1-(5-叔丁基-4-羟基-3-溴苯基)乙酮和3,3-二甲基-5,6-二乙氧基-二氢异吲哚-1-亚胺为主要原料,设计并合成了3个新型的含有偕二甲基结构的PAR-1拮抗剂——1-(3-叔丁基-4-烷氧基-5-取代氨基苯基)-2-(5,6-二乙氧基-3,3-二甲基-1,3-二氢-1-亚胺基-2H-异吲哚-2-基)乙酮氢溴酸盐(2a～2c),其结构经1H NMR和13C NMR表征。TRAP诱导的人血小板聚集活性测试结果表明,2a～2c具有一定的抗血小板聚集作用。     

Total ionizing dose effect in an input/output device for flash memory

Input/output devices for flash memory are exposed to gamma ray irradiation. Total ionizing dose has been shown great influence on characteristic degradation of transistors with different sizes. In this paper, we observed a larger increase of off-state leakage in the short channel device than in long one. However, a larger threshold voltage shift is observed for the narrow width device than for the wide one, which is well known as the radiation induced narrow channel effect. The radiation induced charge in the shallow trench isolation oxide influences the electric field of the narrow channel device. Also, the drain bias dependence of the off-state leakage after irradiation is observed, which is called the radiation enhanced drain induced barrier lowing effect. Finally, we found that substrate bias voltage can suppress the off-state leakage, while leading to more obvious hump effect.     

铜电极在含苯并三唑的硼砂-硼酸缓冲溶液中的光电化学行为研究

用光电化学方法研究了铜电极在含苯并三唑(BTA)的硼砂-硼酸缓冲溶液中的光电化学行为。BTA能使铜电极的光响应由p-型转变为n-型。产生光响应的原因是铜电极表面的Cu2O膜。当BTA存在时由于BTA的作用致使电极表面Cu2O膜中共存着p-型和n-型区域, 电位正移和频率增加导致电极显示n-型光响应。     

Synthesis and Crystal Structure of 2,3,4,6-tetra-O-Acetyl-1-{4-chloro-3-[1-（4-ethoxyphenyl）-1-methylethyl]phenyl}-1-deoxy-β-D-glucopyranose

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system(C31H37ClO10,Mr = 605.06),space group P21 with a = 11.882(5),b = 10.106(5),c = 13.816(6),V = 1545.9(12)3,Z = 2,Dc = 1.300 g/cm3,F(000) = 640,μ = 0.179 mm-1,the final R = 0.0430 and wR = 0.0595 for 4960 observed reflections(I > 2σ(I)).The title compound was confirmed to be a β-anomer by single-crystal X-ray diffraction and 1H NMR.The proximal benzene ring is nearly orthogonal to the glucopyranoside ring,and the two benzene rings are also almost orthogonal to each other.Four non-classical intermolecular hydrogen bonds observed in the crystal lattice help to stabilize the crystal.     

液相色谱-串联质谱法测定21种植物源性食品中茚虫威残留

建立了玉米、花生、核桃、大豆油、绿茶、葡萄、韭菜、香菇以及花椒等21种植物源性食品中茚虫威残留的液相色谱-串联质谱检测方法。样品经乙腈(植物油经正己烷-乙腈)提取,谷物、油料、坚果和植物油采用凝胶渗透色谱(GPC)净化,茶叶采用固相萃取(SPE)净化,水果、蔬菜、食用菌和香辛料采用N-丙基乙二胺(PSA)、十八烷基键合硅胶(C18)、石墨化碳黑(GCB)分散固相萃取剂(d SPE)净化,C18色谱柱分离,0.1%甲酸-乙腈(30∶70)作为流动相进行等度洗脱,质谱采用电喷雾正离子(ESI+)模式电离,多离子监测模式(MRM)定性,基质标准曲线外标法定量。茚虫威的响应值与其浓度呈良好的线性关系,相关系数(r2)大于0.993。在3个加标浓度下,茚虫威的平均回收率为73.7%~115.2%,相对标准偏差不大于13.1%,方法的定量下限为1.5~9.5μg/kg,该方法可满足茚虫威残留分析的要求。     

含反式环己烷结构的C-葡萄糖苷类SGLT2抑制剂的设计、合成与降血糖活性研究

设计并合成了一系列含有反式环己烷结构的C-葡萄糖苷类SGLT2抑制剂,关键步骤是对溴苯甲醚与反式环己烷甲酰氯在无水AlCl3催化下的区域选择性Friedel-Crafts酰基化.所有化合物的结构经过了1H NMR和HRMS的表征.小鼠口服糖耐量实验(OGTT)显示,化合物11a～11d均显示较强的降血糖活性,且11c的活性超过了阳性对照药dapagliflozin,具有良好的开发前景.     

方形基础底板与地基接触应力分布及其表示函数的特性分析

分别从对称和反对称荷载作用下构造出四边自由方形基础底板与地基接触应力分布的函数表达式,通过有限元分析软件ANSYS进行数值模拟。根据有限元数值解与接触应力函数的拟合结果,说明所提出的接触应力函数能较好的反映实际接触应力分布,而且适合不同宽高比的基础底板。