克林霉素磷酸酯的波谱学研究

克林霉素磷酸酯是临床上广泛使用的一种抗菌类药物. 本文对克林霉素磷酸酯进行了¹H、¹³C、³¹P NMR检测,通过DEPT、¹H-¹H COSY、¹³C-¹H HSQC、¹³C-¹H HMBC等2D NMR技术对该化合物的¹H、¹³C谱的信号进行了全归属,并结合量子化学计算和NOESY谱证实了化合物的立体结构. 另外,对克林霉素磷酸酯的飞行时间质谱(TOF-MS)的裂解途径进行了分析.     

注射用针剂药物的拉曼散射光谱研究

本文从药品鉴别的角度出发,首先论述了拉曼光谱分析技术并测试了九种针剂药品的拉曼光谱,通过分析讨论相关药品的拉曼光谱得出了几点结论:(1)某些药品的拉曼峰较多,特征峰值较强,频移范围比较广,例如:氟尿嘧啶,依托泊苷,异烟肼,克林霉素磷酸酯。(2)某些药品拉曼峰较弱,或是没有明显的特征峰,例如:硫酸阿米卡星,甲氧苄啶,利巴韦林,葡萄糖依诺沙星,硫酸庆大霉素。(3)在分析频率及其相对强度时发现,在某一频率下正对的峰高和面积较大,则其相对强度较大,例如:氟尿嘧啶,异烟肼,硫酸阿米卡星,甲氧苄啶,葡萄糖依诺沙星。虽然得到的结论还不能满足对药品的品质鉴定,但通过拉曼光谱分析技术在药品鉴别中的应用,给出了一些药品的拉曼特征谱,为药品的鉴别提供了参考依据。可以说利用光谱分析技术对药品进行鉴别是完全可行的。     

水性丙烯酸聚氨酯涂料中反应性缓蚀剂掺入及其耐蚀性能

利用磷酸和双酚A环氧树脂反应得到功能性缓蚀剂羟基环氧磷酸酯(HEP). 将其添加到水性羟基丙烯酸树脂中,再与水性异氰酸酯固化剂交联,制备了水性羟基环氧磷酸酯/丙烯酸聚氨酯复合涂层(HEP-APU). 由于磷酸酯基团可以与金属基体发生反应,在金属表面形成一层磷化膜,极大的提升了金属的抗闪蚀能力. 利用电化学阻抗谱和极化曲线研究HEP-APU复合涂层对Q235碳钢在3.5wt% NaCl溶液中耐蚀性能. 结果表明,HEP-APU涂料对Q235碳钢具有优越的钝化和耐腐性能,且当HEP在水性丙烯酸聚氨酯涂料中质量分数为0.5%时,所得到的复合涂层的防腐性能最佳.     

荧光法检测磷酸酯液压油外泄漏平台设计与实现

通过采用LS-55型荧光分光光度计对HyJet Ⅴ磷酸酯液压油以及Jet Oil Ⅱ、2197润滑油的荧光特性进行分析,提出了一种采用荧光法来检测磷酸酯液压油外泄漏的方法.通过选取合适的光源、滤光片、倍增管等器件,搭建了磷酸酯液压油外泄漏检测平台.并且通过实验验证了平台的可行性,为荧光法检测磷酸酯型液压油外泄漏的实际应用奠定了基础.     

31P核磁共振谱应用数则

用³¹P对烷基膦酸二烷基酯,乙酰丙烯磷酸二烷基酯的组成进行了分析,为寻找反应条件和产品纯化方法提供了有益的数据。并对几种腺嘌呤核苷酸磷酸酯及磷酰胺不同的立体异构体进行了测定,平展式较直立式在高场约2ppm处共振。     

多甘醇-磷酸酯-EDTA酯共聚物铁(Ⅲ)配合物的合成和磁共振成象增强作用

通过乙二胺四乙酸双酸酐、二氯磷酸酯与多甘醇共缩聚，制得一系列三元共聚物配体．用配体与三氯化铁反应，得到相应的铁配合物．表征了配体和配合物的化学结构，测试了配合物的纵向弛豫速率，并考察了配合物的急性毒性和磁共振成象增强作用．     

阿奇霉素含量的荷移光谱法测定

用分光光度法分别研究了阿奇霉素与7,7,8,8-四氰基对二次甲基苯醌(TCNQ)和氯冉酸(CL)之间的荷移反应。实验表明：阿奇霉素与TCNQ间的反应在丙酮介质中进行,形成的络合物在743和842 nm有两个吸收峰,表观摩尔吸光系数分别是2.7×104 L·mol-1·cm-1和5.0×104 L·mol-1·cm-1;阿奇霉素与氯冉酸的反应在丙酮介质中进行,形成的络合物在530 nm处有吸收峰,表观摩尔吸光系数2.4×103 L·mol-1·cm-1。用摩尔比法和等摩尔连续变化法测得荷移络合物中阿奇霉素与配体的摩尔比均为1∶2。用以上两种方法测定了阿奇霉素片剂中阿奇霉素的含量,相对标准偏差为1.0%～1.4%(n=6),回收率为97%以上,与标准方法比较结果准确。     

一种新型的喹啉-4-氨基磷酸酯衍生物的波谱学研究

以2-苯基-4-喹啉酮为原料,通过磷酰化反应将磷酰氮芥引入到2-苯基-4-喹啉酮中,合成了一种新型的喹啉-4-氨基磷酸酯衍生物. 应用DEPT、¹H-¹H COSY、¹³C-¹H HSQC、¹³C-¹H HMBC等2D NMR核磁共振技术,对该化合物的¹H、¹³C NMR谱的信号进行了全归属;通过飞行时间质谱(TOF-MS)对这种新型的喹啉-4-氨基磷酸酯衍生物的裂解途径进行了分析.     

利用荧光法检测磷酸酯液压油的泄漏

提出了一种检测飞机液压油泄漏的方法--荧光法,以美孚磷酸酯液压油为例,实验验证了荧光法检测磷酸酯液压油泄漏的可行性。采用LS-55型荧光分光光度计以及实验室搭建系统对HyJet Ⅴ磷酸酯液压油以及Jet Oil Ⅱ、2197润滑油的荧光特性进行了分析。研究结果表明,可以用不同荧光发射光谱峰值来区分三种油,荧光法检测磷酸酯液压油泄漏是可行的。该技术可实现对飞机液压油泄漏的实时、在线、现场测量。     

FTIR跟踪研究不饱和氯代阻燃聚醚多元醇与亚磷酸酯阻燃剂的反应

采用FTIR技术跟踪研究了由乙二醇和环氧氯丙烷以及烯丙基缩水甘油醚共聚而成的不饱和氯代聚醚多元醇,与亚磷酸三甲酯发生酯交换反应和酯交换聚合反应以及Arbuzov重排反应过程,合成反应型聚醚多元醇亚磷酸酯阻燃剂的方法。实验考察了物质量配比、反应温度、投料方式等对上述反应进程的影响。分析结果表明反应温度是决定上述反应进程的关键因素,同时适当条件下合成的反应产物,可以用作一种光固化的兼有抗老化和增塑功能新型有机磷酸酯阻燃剂。     

Isotopic Exchange Between Barium Oxalate and Barium Ion in Aqueous Solution

The heterogeneous isotopic exchange reaction of precipitated barium oxalate in barium chloride solution has been studied using Ba-133 as tracer. The effect of barium chloride concentration on the rate of isotopic exchange reaction has been studied. It was found that the rate was controlled by surface mass reaction and particle diffusion process in the solid particle. The result also indicate that the effect of recrystallization can be neglected.     

激光磁共振方法研究异戊二烯与NOx的化学反应

以激光磁共振为手段分别在紫外照射和火花放电条件下观测到异戊二烯与ＮＯ／ＮＯ２的反应，所获得的信息对了解大气化学反应及光化学烟雾有着重要的意义。     

配合物PdCl_2[(PPh_2)_2CHC1]的合成、结构及反应机理

合成了新配合物PdCl2[(PPh2)CHCl]，用核磁、红外光谱、元素分析等表征了其结构，X－rax衍射确定了单晶结构.应用电子顺磁共振-自旋捕获（EPR－ST）对技术研究了其反应的机理．捕获到PPh2及含碳自由基中间体，提出了反应机理．     

Pd(OAc)2与PPh3在氯代甲烷中的反应研究

用Pd(OAc)₂与PPh₃在四氯甲烷中反应,合成了配合物PdCl₂(PPh₃)₂?CCl₄,得到单晶,用X-ray衍射确定了单晶结构.应用电子顺磁共振-自旋捕获(EPR-ST)技术研究了其反应的机理.捕获了含碳自由基中间体,提出了反应机理.     

荷移分光光度法测定罗红霉素

本文研究确定了罗红霉素与甲酚红的荷移反应条件。在乙醇 丙酮介质中 ,罗红霉素与甲酚红在35℃的温度时发生荷移反应 ,产物的最大吸收波长为 456nm ,表观摩尔吸光系数为 1 0 5× 1 0 4L·mol- 1 ·cm- 1 ,罗红霉素的浓度在 0～ 80mg·L- 1 范围内与吸光度呈线性关系 ,相对标准偏差为 0 87% (n=6) ,回收率在 98%以上。测定了荷移络合物的组成比为 1∶1 ,探讨了反应机理 ,其中罗红素作为电子给予体、甲酚红作为电子接受体发生了电荷转移反应。     

重丰中子新同位素——238Th

利用兰州重离子加速器（ＨＩＲＦＬ）提供的６０ＭｅＶ／ｕ的１８Ｏ离子束照射天然铀靶,通过多核子转移反应生成２３８Ｔｈ．用快速放射化学分离技术从铀及其反应产物的混合物中分离出Ｔｈ同位素．使用两台高纯锗（ＨＰＧｅ）探测器测量了样品的γ射线活性,观测到了２３８Ｔｈ的β－衰变子体２３８Ｐａ的γ射线的生长、衰变行为,测定２３８Ｔｈ的半衰期为9.4±2.0min A new nuclide 238Th has been produced via multinucleon transfer reaction by 60 MeV/u 18 O ion irradiation of natural uranium. The produced thorium was radiochemically separated from the mixture of uranium and its reaction products. The activity of thorium was measured by using a HPGe detector and a planar HPGe detector. 238 Th has been identified for the first time by measuring the growth and decay of the γ rays from its daughter nucleus 238 Pa.     

A sol-gel method for preparing ZnO quantum dots with strong blue emission

ZnO quantum dots (QDs) with strong blue emission have been successfully synthesized by sol-gel method, and their crystal structures, sizes, and photoluminescence properties were characterized by X-ray diffractometer, scanning electron microscope, and ultraviolet-visible spectroscopy. It has been found that ZnO QDs had a hexagonal wurtzite crystal structure, and their average diameter was about 16.0-32.2 nm. Both the reaction time and temperature were found to have a strong influence on the average size and photoluminescence properties of ZnO QDs. Longer reaction time and higher reaction temperature resulted in larger average size for ZnO QDs. It has been shown that at reaction temperature 60 °C the emission intensity for ZnO QDs increased first with reaction time before 7 h and then decreased after 7 h. For the same reaction time 7 h, ZnO QDs synthesized at 60 °C showed the strongest emission intensity. It was found that annealing in nitrogen, vacuum, and air all resulted in an increase of the size of ZnO QDs and a reduction in their photoluminescence. The dependence of the size and properties of ZnO QDs on the reaction parameters as well as the annealing conditions has been discussed.     

Ultrasound mediated alkaline hydrolysis of methyl benzoate--reinvestigation with crucial parameters

In the present work hydrolysis of methyl benzoate was carried out using aqueous sodium hydroxide solution at room temperature in the presence of ultrasound since otherwise the same reaction takes place at relatively high temperature. Also, the above hydrolysis reaction was investigated at a relatively larger scale with the variation in parameters influencing the emulsification process and hence the reaction rates. It has been observed that the position of ultrasound source on the liquid-liquid interface is a crucial parameter affecting the two-phase emulsification rates. The poor bulk mixing occurring in the presence of ultrasound alone with an increase in the volume of the reaction mixture and its consequent effect on the reaction kinetics has been conclusively established. These studies have shown that the use of ultrasound with mechanical stirring can result in substantial reduction in the overall power consumption, especially for reaction systems like hydrolysis that do not require very high temperatures and pressures generated by cavitation.     

Knoevenagel reaction in water catalyzed by amine supported on silica gel

Summary An environmentally benign and sustainable Knoevenagel reaction of aldehyde with ethyl cyanoacetate has been achieved at ambient temperature in water employing 3-aminopropylated silica gel (NAP) as a catalyst. Wide applicability of the reaction is illustrated by the results that not only arylaldehydes of both electronic characters but also aliphatic aldehydes afforded the products. The reaction condition was so mild that aldehydes having acid- or base-sensitive substituents provided substituted α-cyano-α, β-unsaturated esters. The catalyst has been efficiently recycled more than five times without any pre-treatment. Catalyst loading was successfully reduced to 0.0029 mmol% (TON = up to 9,226). This protocol was also applicable to the Knoevenagel reaction of malononitrile in good yields in water.     

Hyperfine interactions in solid state reaction of hematite with aluminium

The solid state reaction of hematite with aluminium has been induced by mechanical alloying. Mössbauer spectroscopy and X‐ray diffraction have been used to investigate the reaction products. The reaction was completed in a time longer than 15 min but shorter than 30 min. During the reaction a Fe(Al) bcc solid solution was obtained as a matrix, with Al₂O₃ as reinforcement. After prolonged milling both components were in a nanocrystalline paramagnetic state.