L-羟脯氨酸寡肽混合物的高效液相色谱分离与质谱分析

研究了三氯氧磷辅助下L-羟脯氨酸的成肽反应,建立了采用反相高效液相色谱-质谱/质谱联用技术分离鉴定羟脯氨酸寡肽混合物的方法,优化了L-羟脯氨酸寡肽混合物的色谱分离条件。实验以YWG C8柱(10μm,250mm×10mm)为分离柱,以乙腈-0.06%三氟乙酸水溶液(体积比为2∶98)为流动相进行等度洗脱,在正离子模式下对洗脱物进行了电喷雾电离串联质谱鉴定。结果显示,分离出的各组分分别为L-羟脯氨酸二肽、L-羟脯氨酸环二肽和L-羟脯氨酸三肽

高粱子粒淀粉表面色素的树脂分离研究

对纯化高粱淀粉过程中所得到的淀粉共生天然色素进行了树脂分离纯化研究。得到了树脂分离高粱淀粉共生色素的吸附动力学结果,3 种大孔吸附树脂 HPD-600、AB-8、H103 对高粱红的吸附为慢速平衡型。通过对树脂分离所得色素成份的红外光谱、紫外光谱、质谱分析得出,高粱籽粒淀粉共生色素与高粱壳中的高粱红主要成份是同样的物质,鉴定出所分离的主要成份之一为 5,7,4′-三羟基黄酮

Progress in the Atherton-Todd reaction and its stereochemical mechanism

本文总结了近几十年来对含有P-H键的四配位和五配位磷化合物的ATHErTOn-TOdd反应的研究,尤其对其立体化学反应机理研究进行了详尽的叙述.自发现ATHErTOn-TOdd反应之后,虽然对其反应机理进行了几十年的研究,但前期工作主要集中在反应中间体的研究.直至近十几年来,才分别对含有P-H键的四配位和五配位磷化合物的ATHErTOn-TOdd反应的立体化学机理进行了较详细的研究,但至今仍缺乏对其立体化学机理全面的综述和介绍,希望本文可以弥补文献不足,不仅对ATHErTOn-TOdd反应有个客观全面的介绍,而且对于其立体化学反应机理的研究也进行详细的综述.对于ATHErTOn-TOdd反应立体化学机理的深入研究将有助于设计合成新型的具有光学活性的四配位和五配位磷手性中心的化合物.In this review, we summarize the literatures in the latest decades on the Atherton-Todd reaction of the tetracoordinated and pentacoordinated phosphorus compounds containing P?H bond.Especially, the review focuses on the development of the stereochemical mechanism of the Atherton-Todd reaction.Although the reaction mechanism has been investigated for decades after the discovery of the reaction, the earlier studies mainly concentrated on the reaction intermediate.Up to the past dozen years, the stereochemical mechanism of the Atherton-Todd reaction was studied in detail.However, up to now, there is few review and introduction to the stereochemical mechanism of the AthertonTodd reaction.We hope this article could compensate for this limitation, and it not only summarizes the general Atherton-Todd reaction, but also introduces the recent research results on the stereochemical mechanism.It is considered that the further investigation on the stereochemical mechanism of the Atherton-Todd reaction will be helpful to design and synthesize the novel tetracoordinated or pentacoordinated compounds with phosphorus chiral centers.国家自然科学基金(21172201;20672104)的资

Study of the Interaction Between Polar Dipeptides and Metal Ions by NMR

利用核磁滴定法研究了极性链状二肽(均为ll构型)与金属离子之间的相互作用.极性二肽在与一价金属离子相互作用时,两者间的化学计量比为1∶1,并求得lI+与10种极性二肽结合常数的大小,其中与l-glu-l-glu的结合常数最大,这可能与l-glu-l-glu含有较多的富电子原子有关.在此基础上又研究了Cu2+,zn2+,CO2+3种二价金属离子与极性二肽间的相互作用,结果表明,二价金属离子与二肽间的相互作用是通过两步完成的.The interactions of 10 polar chain dipeptides( L-L configuration) with metal ions were examined by NMR.These polar chain dipeptides exhibited a tremendous selectivity toward monovalent mental ion,showing a stoichiometric binding with 1∶ 1,and the association constants of dipeptides with Li+were acquired.The results showed that L-Glu-L-Glu had stronger binding ability toward Li+ions than other dipeptides,and suggested the electron-rich atoms in L-Glu-L-Glu molecular were favorable for the interaction with metal ions.Furthermore,the interactions of divalent metal ions( Cu2 +,Zn2 +,Co2 +) with 10 polar chain dipetieds were studied,which implied the interaction between them was carried out in two stages.国家自然科学青年基金资助项目;编号2110509

钙基脱硫剂固硫率的测定方法

介绍了钙基脱硫剂固硫后形成的 Ca O-Ca SO4 固体混合物中钙和硫酸根的测定方法。改进了文献中微量硫酸根的滴定分析 ,分析了滴定过程的机理。先用高氯酸将固体混合物溶解形成水溶液 ,然后以钍试剂为指示剂 ,用高氯酸钡溶液滴定溶液中的微量硫酸根 ,并用 EDTA法以钙红为指示剂滴定溶液中的钙离子 ,从而可以计算出钙基脱硫剂的固硫率 (表示为脱硫后固体混合物中的钙硫化 )