戊烯自由基阳离子的密度泛函理论研究

使用密度泛函理论B3LYP方法和6-31G(d,p)、6-31＋G(d,p)、6-311G(d,p)及6-311＋G(d,p)基组，分别对2-C5H10＋和1-C5H10＋的各种构象进行了几何构型优化，并用B3LYP/6-311G(d,p)进行了频率分析计算.计算预言1-C5H10＋具有非平面构型，与以往报导的从头算计算结论相反.在两个自由基阳离子的各种构象的B3LYP几何构型上，进行了B3LYP和UMP2(full)方法的超精细偶合常数计算，得到了比以往更好的结果.     

Liquid Chromatography-Electrospray Quadrupole Linear Ion Trap Mass Spectrometric Method for Quantitation of Domperidone in Chinese Healthy Volunteers

A rapid,sensitive,and accurate method based on LC/MS/MS was developed and validated for the determination of domperidone in human plasma.Domperidone and internal standard,tramadol,were extracted from plasma with diethyl ether-dichloromethane(60∶40,volume ratio)and separated by reversed-phase HPLC with methanol-water-ammonia solution(80∶20∶0.2,volume ratio)as the mobile phase.Detection was carried out via multiple-reaction monitoring(MRM)on a Q-trapTM LC/MS/MS system(Q-trapTM).The assay result was linear over a concentration range of 0.1-30 ng/mL with a limit of quantitation(LOQ)of 0.1 ng/mL.The inter-and intra-day precision levels were within 7.52% and 12.9%,respectively,whereas the accuracy was within a range of 87.3%-114%.This method has been successfully applied to evaluate the pharmacokinetics of domperidone in Chinese healthy volunteers given an oral dose of 10 mg.     

Characterization and separation of Al_(13) species using gel-filtration chromatography

Polyaluminum chloride (PAC) coagulant has been developed and widely used in water and wastewater treatment industry since the 1980s[1]. PAC is normally made by partial hydrolysis of acid aluminum chloride solution using slow alkaline titration method. However, this method would result in many different Al species. Among these Al species, it seems that tridecamer (Al13O4(OH) 724 , often denoted by Al13) is the most effective and stable polymeric Al species for water and wastewater treatme…     

Quantitative Determination of Oxalic Acid Using Victoria Blue B Based on a Catalytic Kinetic Spectrophotometric Method

A sensitive catalytic method is developed for the spectrophotometric determination of oxalic acid. The procedure is based on the effect of oxalate on the oxidation of Victoria blue B by dichromate in dilute sulfuric acid medium. The reaction is quantitatively estimated by measuring the decrease in absorbance of Victoria blue B at the maximum wavelength of 610nm after quenching the reaction with tap water. The factors effecting the sensitivity and reproducibility of the reaction were studied. The method is not interfered with by foreign species generally associated with oxalate and oxalic acid. The described method is simple, specific, inexpensive and suitable for oxalic acid concentrations of between 0.06 and 9.0µgmL^–1. It was validated with satisfactory results by determining oxalic acid content in water extracts from plant materials such as spinach and Lathyrus sativus.     

脱乙酰壳多糖化学修饰电极测定铂的研究

用脱乙酰壳多糖修饰电极为工作电极，阳极溶出伏安法测定痕量铂。在ｐＨ＝２￣３的ＫＣｌ－ＨＣｌ底液中，－０．３Ｖ富集２ｍｉｎ，静止１５ｓ，以０．２Ｖ／ｓ扫速阳极溶出，峰电位在－０．１６Ｖ（ｖｓ．ＳＣＥ），铂（Ⅳ）离子浓度在０．５￣５．０μｇ／ｍＬ范围内与峰高呈线性关系。富集１０ｍｉｎ后，可检测０．０２５μｇ／ｍＬ铂（Ⅳ）。该法用于贵金属矿样的测定，无需分离，结果满意。用循环伏安法、紫外光谱和拉曼光谱研     

4,4'-[(2,2-二苯乙烯)-1,1-双(4,1-亚苯基)]二吡啶的合成、表征及其聚集诱导发光性能研究

以提升学生的实验操作及创新能力为目的的综合化学实验，采用简单的2步法（缩合和Suzuki反应）合成了一种具有聚集诱导发光性能的化合物4，4'-[（2，2-二苯乙烯）-1，1-双（4，1-亚苯基）]二吡啶（简称2Py-TPE）。利用过滤、洗涤、萃取、干燥和柱层析等常用的有机分离操作手段对该化合物进行纯化；使用核磁共振仪、高分辨质谱仪、红外光谱仪及稳态瞬态荧光光谱仪对其进行结构表征和聚集诱导发光性能研究。该实验不仅可以促使学生了解以四苯乙烯衍生物为代表的聚集诱导发光材料的研究现状，而且能够培养学生的综合实验能力和科学探究能力。     

HEMA-NVP-St三元共聚体系研究Ⅲ.均化剂对共聚物组成均一性的影响

用溴化钾-溴酸钾滴定法测定双键含量,元素分析法测定共聚物组成。讨论了HEMA-NVP-St三元共聚体系在不同反应程度时共聚物组成的变化,以及在此三元共聚体系中引入均化剂后,少量均化剂对共聚体系组成均一性的影响。发现在HEMA-NVP-St三元共聚体系中加入均化剂,对共聚反应的反应动力学影响不大,但对共聚物的组成均一性有较大影响。它的加入使三元共聚物中的链节比分布(即不同反应程度时,产物的累积平均组成)向较均一的方向发展。结合红外光谱、电子显微镜等实验证据,从微观结构上探讨了约化剂的作用。阐明均化剂改善了反应体系的相容性,从而得到组成分布较为均一的共聚产物。     

固相萃取-气相色谱-高分辨质谱法测定巢湖水中半挥发性有机化合物

描述了巢湖水中半挥发性有机化合物的提取、测定过程和初步结果。湖水中半挥发性有机化合物的提取采用XAD-2和XAD-4混合树脂富集，用气相色谱-高分辨质谱法测定了所萃取的有机化合物，并给出相应的分子式和结构式。春季湖水中检测到14种有机化合物。     

萜品油烯的DeMayo光环加成产物的反应研究

通过萜品油烯和2，6-二氧代戊酸甲酯的de Mayo反应，使[2 + 2]环加成产物 3-6经retro-aldol重排，开环生成取代环己烯7和12。在不同反应介质中对开环产 物进行再环合，并对其反应机理进行研究。在碱性条件下，经分子内Claisen缩合 反应形成螺环化合物；以对甲本碘酸为催化剂的环合，除生成正常的Claisen缩合 产物以外，7和12均发生烯键亲核加成反应，生成具有二环[3.3.1]结构的桥环化合 物9-11和二环[3.2.1]结构的桥环化合物16-18。所得新化合物的化学结构均经IR, ~1H NMR，~(13)C NMR及元素分析予以确定。     

GC/MS法分析油松节挥发油化学成分

用气相色谱-质谱法对山东昆嵛山产油松节挥发油进行化学成分的分析。采用水蒸气蒸馏法从油松节中提取挥发油。采用不同类型的毛细管柱进行分析，找出最佳分析条件，用归一化法测定其含量，并用气相色谱-质谱法对化学成分进行鉴定。共鉴定了48个成分，占挥发油总成分的84％以上。结果表明，此方法稳定可靠，重现性好，适用于中药挥发油的化学成分分析。