免疫亲和净化-超高效液相色谱串联质谱法同时测定猪肉和鸡蛋中的12种磺胺类药物

建立了猪肉和鸡蛋中12种磺胺类药物的免疫亲和净化-超高效液相色谱串联质谱的确证方法。样品用超声提取后,直接过磺胺类药物免疫亲和净化柱净化;氮气吹干后用1∶9（v/v）的甲醇/水溶液定容,超高效液相色谱-串联质谱（UPLC-MS/MS）测定,电喷雾正离子（ESI+）、多反应模式下监测;实验结果表明,样品中磺胺类药物浓度在10～200μg/kg范围内时与其峰面积成良好线性关系,仪器检出限为0.4～2.0μg/L,方法的检出限为1.0～5.0μg/kg,3个加标水平下平均回收率为67%～100%,相对标准偏差为0.9%～10.0%,符合痕量分析的要求。      

Development of Novel Quinoline-Based Sulfonamides as Selective Cancer-Associated Carbonic Anhydrase Isoform IX Inhibitors

A new series of quinoline-based benzenesulfonamides (QBS) were developed as potential carbonic anhydrase inhibitors (CAIs). The target QBS CAIs is based on the 4-anilinoquinoline scaffold where the primary sulphonamide functionality was grafted at C4 of the anilino moiety as a zinc anchoring group (QBS 13a–c); thereafter, the sulphonamide group was switched to ortho- and meta-positions to afford regioisomers 9a–d and 11a–g. Moreover, a linker elongation approach was adopted where the amino linker was replaced by a hydrazide one to afford QBS 16. All the described QBS have been synthesized and investigated for their CA inhibitory action against hCA I, II, IX and XII. In general, para-sulphonamide derivatives 13a–c displayed the best inhibitory activity against both cancer-related isoforms hCA IX (K_Is = 25.8, 5.5 and 18.6 nM, respectively) and hCA XII (K_Is = 9.8, 13.2 and 8.7 nM, respectively), beside the excellent hCA IX inhibitory activity exerted by meta-sulphonamide derivative 11c (K_I = 8.4 nM). The most promising QBS were further evaluated for their anticancer and pro-apoptotic activities on two cancer cell lines (MDA-MB-231 and MCF-7). In addition, molecular docking simulation studies were applied to justify the acquired CA inhibitory action of the target QBS.     

QuEChERS-高效液相色谱-串联质谱法联用测定鸡肉中磺胺类药物残留

目的建立QuEChERS-高效液相色谱-串联质谱法测定鸡肉中磺胺类药物残留量的分析方法。方法以乙腈为提取溶剂,氯化钠盐析分层,离心后上清液经C18填料萃取净化,用乙腈和0.1%(V:V)甲酸水溶液作为流动相进行梯度洗脱,EndeavorsilC18柱色谱柱进行色谱分离,在高效液相色谱-串联质谱仪上采用电喷雾正离子扫描模式(electrospray ionization, ESI+)检测,外标法定量。结果该方法在5～200μg/L范围内有良好的线性关系, 8种磺胺类药物残留的相关系数均大于0.99,方法检出限在3～6μg/kg范围,定量限在10～20μg/kg范围。分别在3个浓度水平20、100、300μg/kg加标,平均回收率在75.6%～115.2%范围,相对标准偏差在1.9%～12.4%范围。结论本方法操作简便,准确度和精密度好,可快速检测鸡肉中磺胺类药物的残留量。     

PZ活化MDEA乙烷深度脱碳工艺研究

目的 解决醇胺法乙烷脱碳工艺造成的乙烷损失量较大和装置能耗较高等问题。方法 用Aspen HYSYS软件对某乙烷回收流程的粗乙烷产品进行胺法脱碳模拟,在控制乙烷损失物质的量比小于0.3%的情况下对胺液中的PZ和MDEA质量分数进行了优选,同时对乙烷脱碳流程进行能耗优化。结果 与天然气脱碳工艺不同,乙烷脱碳工艺的MDEA质量分数太高会损失大量乙烷。在达到脱碳效果的前提下,较低的MDEA质量分数可避免损失大量乙烷,最佳MDEA质量分数为20%～28%。在此MDEA质量分数的条件下,可保证乙烷损失比仅为0.3%,往胺液中加入少量哌嗪(PZ)就可显著提高胺液对CO₂的吸收效果,最佳PZ质量分数为2.5%～5.5%。乙烷脱碳装置的主要能耗为胺液再生能耗,优化后装置的总能耗显著降低。结论 在工业条件下,应用较低质量分数的胺液可显著降低乙烷损失,可合理提高富胺液入再生塔温度或适当降低脱碳溶液循环量,以降低装置能耗。     

哌嗪合成催化剂研究进展

综述了单一金属催化剂、复合型金属催化剂、分子筛催化剂以及固体酸催化剂在哌嗪合成中的应用,提出开发反应条件温和、可直接得到无水哌嗪的催化剂是哌嗪合成催化剂的研究开发重点.     

1-（4-羟基苯基）-4-（4-硝基苯基）哌嗪的合成概述

三唑类药物是目前抗真菌药的主流,特别是用于治疗深部真菌感染。1-（4-羟基苯基）-4-（4-硝基苯基）哌嗪是其重要的药物中间体,作为新-代抗真菌药关键中间体其的合成已成为研究热点。较全面地介绍了1-（4-羟基苯基）-4-（4-硝基苯基）哌嗪的各种合成路线。其合成途径基本上是先制备单N-芳基取代哌嗪,产物继续和适当的芳基卤化物进行N’-芳基化反应,得到1-（4-羟基苯基）-4-（4-硝基苯基）哌嗪。     

Bridging the Buried Interface with Piperazine Dihydriodide Layer for High Performance Inverted Solar Cells

Given that it is closely related to perovskite crystallization and interfacial trap densities, buried interfacial engineering is crucial for creating effective and stable perovskite solar cells. Compared with the in-depth studies on the defect at the top perovskite interface, exploring the defect of the buried side of perovskite film is relatively complicated and scanty owing to the non-exposed feature. Herein, the degradation process is probed from the buried side of perovskite films with continuous illumination and its effects on morphology and photoelectronic characteristics with a facile lift-off method. Additionally, a buffer layer of Piperazine Dihydriodide (PDI₂) is inserted into the imbedded bottom interface. The PDI₂ buffer layer is able to lubricate the mismatched thermal expansion between perovskite and substrate, resulting in the release of lattice strain and thus a void-free buried interface. With the PDI₂ buffer layer, the degradation originates from the growing voids and increasing non-radiative recombination at the imbedded bottom interfaces are suppressed effectively, leading to prolonged operation lifetime of the perovskite solar cells. As a result, the power conversion efficiency of an optimized p-i-n inverted photovoltaic device reaches 23.47% (with certified 23.42%) and the unencapsulated devices maintain 90.27% of initial efficiency after 800 h continuous light soaking.     

哌嗪改性聚醚基聚二甲基硅氧烷的合成与应用性能研究

利用哌嗪与自制的聚醚／环氧硅油中间体反应合成了一种哌嗪改性聚醚基聚二甲基硅氧烷PPEPS，对其进行了结构表征和应用。结果表明：原料含氢硅油的平均相对分子质量、PPEPS的硅含量对其应用性能有影响。增加原料含氢硅油的平均相对分子质量，提高硅含量，可改善PPEPS的柔软性，而对织物的吸湿性影响不大。     

新型超临界流体色谱仪在磺胺药物分析中的应用研究

采用新型超临界流体色谱仪,在优化条件下于7 min内完成对4种磺胺类药物的分离。考察了色谱填料类型、共溶剂类型、共溶剂比例、背压、流速、柱室温度等条件对样品保留行为的影响。实验结果显示,色谱填料类型对样品保留行为的影响最为明显,正相硅胶柱最适合分离该类药物;共溶剂种类、共溶剂比例及流速对保留行为产生影响,其中甲醇最适用于该样品的分离,共溶剂比例越高、流速越快,洗脱时间也越短;背压和柱室温度的改变对该样品的保留行为影响较小。     

Enantioselective Polymeric Composite Membrane for Optical Resolution of Racemic Mixtures of α-Amino Acids

The optical resolution of racemic mixtures of α-amino acids was performed using novel enantioselective polymer membrane to obtain optically pure isomers. The novel membranes were prepared by polymerizing a mixture of D-arginine, piperazine, and trimesoyl chloride in-situ interfacial on polysulfone ultrafiltration membrane. ATR-FTIR spectroscopy, Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), and Transmission Electron Microscopy (TEM) techniques were used to characterize the membranes and co-relate membrane morphology with membranes performance. The optical resolution performance of the membrane process was quantified by performing optical resolution of racemic arginine and asparagine in pressure driven separation mode at low pressures. The influence of monomers concentrations and their ratio in the polymerizing mixture on the flux and enantioseparation was studied. The observations indicated >91 percent enantiomeric excess (>91% ee) of L-arginine and >56 percent enantiomeric excess (>56% ee) of L-asparagine in the permeate of the racemic feed. The membrane prepared using equiconcentrated (2%) solutions of D-arginine, piperazine, and trimesoyl chloride exhibited highest enantiomeric excess (91%). At 91% ee the separation factor (α) for L-arginine was approximately 16.