分析化学实验课程教学大纲的标准化改造与构建

基于工程教育专业认证标准的要求,结合专业课程的特点,对我校制药工程专业的分析化学实验教学大纲进行了标准化改造。标准化的教学大纲更加突出了专业适用性,关联了教学要求与教学内容和考核评定,增加了考核量化指标与课程持续改进的方式,进一步规范了分析化学实验课程的教学。标准教学大纲的构建为实验教学活动提供了更加明确的指导,有利于缩小不同教师教学的差异性,保证了实验教学的质量,为建立可持续完善的工程类实验教学标准体系提供了具体参考。     

储氢合金电极的表面修饰研究

利用等离子体技术对AA型MH/Ni电池的储氢合金电极进行了镀覆导电膜层的表面修饰,用XRD及SEM对电极结构进行了表征.极片经过表面修饰的电池,其内阻降低了24％,放电容量有了明显提高,5C (7.5 A) 放电容量提高了200 mA•h,放电平台电压提高了约0.14 V,导电膜层还起到了电极保护层的作用,抑制了合金的粉化,提高了电池的循环稳定性.同时,电池内压显著降低,电池性能有了较大改善.     

农林高校基础化学多层次课程体系和教学内容的改革与实践

以农林高校基础化学课程体系和教学内容改革为抓手,构建了农科特色鲜明的多层次课程体系,优化设计了教学内容,增强了教学的针对性,突出了学生个性的发展,为农科院校创新人才的培养奠定了重要的化学基础。     

促进学生认识发展的“电离和离子反应”专题的单元整体教学研究

系统梳理了电离、离子反应专题的已有研究,分析了电离、离子反应内容对学生认识发展的作用,进而确立了化学1模块电离、离子反应专题的教学论问题并进行了阐述分析。在上述研究的基础上,设计了化学1模块电离、离子反应专题的单元整体教学,并进行了教学实践,取得了较好的教学效果。     

前言

自20世纪初期,德国化学家EmilFischer首先合成了甘氨酸二肽片段,并第一次提出“peptide”（多肽）这一名词,多肽化学的研究已经历了100多年的发展．1953年,Vigneand小组首次完成了生物活性肽催产素的合成,并因此于1955年获得了诺贝尔化学奖．1963年,Merrifield提出了多肽固相合成法,并发明了第一台多肽自动合成仪,大大简化了多肽合成的流程、提高了合成的效率,从而促使多肽化学实现了飞跃式发展,Merrifield也因此获得了1984年诺贝尔化学奖．1965年,我国科学家完成了牛结晶胰岛素的合成,     

基础化学实验室的建设与管理

化学实验室是全面完成化学教学任务的重要基地。 我院2002年建立了设备比较先进的化学实验室,给学生创造了良好的实验条件,并进行了科学化的管理,规定了各种规章制度和有关职责,较好地完成了化学教学任务。在实践中。采取：固定优秀代课教师兼管,勤工助学学生帮忙的管理办法,既减轻教师的劳动强度,又培养了学生的技能,且协调了各种关系,有利于化学教学质量的提高。     

非理想气体的逸度因子和非理想溶液的活度系数

对单组分非理想气体,推导了它的逸度因子的微分方程式。对多组分非理想气体,推导了各组分逸度因子满足的微分方程式,定义了一个总逸度因子,并找到了总逸度因子和各组分逸度因子之间的关系。同样,对非理想溶液,推导了各组分活度系数满足的微分方程式,定义了非理想溶液的总活度系数,并找到了两者满足的关系。最后分析了逸度因子和活度系数之间的异同点。     

酰胺基团对Gemini表面活性剂表面活性和聚集行为的影响

本文合成了含酰胺基团和不含酰胺基团的两类Gemini阳离子表面活性剂,测定了其表面活性参数,研究了酰胺基团对表面活性剂的表面活性和聚集行为的影响。结果表明,酰胺基团提高了Gemini阳离子表面活性剂的临界胶团浓度,降低了胶团聚集数,增强了胶团微极性,增大了表面活性剂的饱和吸附量。     

共聚反应单体竞聚率测定实验的设计与实践

通过实际教学情况,设计实施了共聚反应单体竞聚率测定的设计性教学实验,并以核磁共振的方法进行结果测定。通过实验教学,学生掌握了温度变化对竞聚率影响的实验方法,提高了理论联系实际的能力,使抽象理论实际化,让学生初步建立起抽象与具体的联系,并且充分拓展了学生的视野和思维。在增加了实验趣味性的同时也优化了教学方式和课程体系,取得了良好的教学效果。     

食品安全与健康——深圳市卫生部门食品安全保障体系

回顾了国际国内的食品安全问题以及管理现状,着重介绍了深圳市卫生部门食品安全保障工作.近几年,深圳市有效运行了食品污染物监测网络,基本掌握了食品安全存在的问题,通过对问题食品的追溯,从根本上着手解决问题,控制了污染食品进入餐桌;以风险评估作为科学手段,做好重点食品污染物的监测预警;引导和提醒消费者提高自我保护意识,为政府制定相关决策提供了依据,从而显著地减少了食源性疾病的发生,有效地保障了公众的身体健康.     

一种新型超临界流体萃取-高效液相色谱在线联用系统的构建

天然产物研究一直是植物学、化学和药学的重要研究领域．通过从天然产物中寻找生物活性成分和先导物是创制新药的有效途径之一．有效成分的提取是天然产物研究中最基本和最关键的环节．超临界流体萃取（Supercritical fluid extraction,简称SFE）是近年来发展较快的一种新型样品提取技术．超临界CO2作为最常用的萃取剂已被用于天然药物中非极性和弱极性有效成分的提取,尤其是挥发性和热敏性的物质．此外,通过加入适当的添加剂还可有效地萃取极性化合物,和传统的化学方法相比,     

复杂基体中痕量多环芳烃分析测定方法的研究进展

介绍了环境样品（水和土壤）以及植物油中痕量多环芳烃的分析检测方法。对样品的预处理过程和分析方法做了评价。采用一些新的预处理方法（包括液相色谱法、固相萃取法、超临界二氧化碳萃取法）,并结合色谱-质谱在线联用分析检测方法能够获得比较理想的分析结果。引用文献52篇。     

Selective extraction of astaxanthin from crustaceans by use of supercritical carbon dioxide

An on-line supercritical fluid extraction (SFE) system coupled to a continuous flow manifold including a UV detector was used as a screening system to extract astaxanthin from crayfish, which was found to be the major carotenoid present in the samples. This compound constitutes the principal additive used to dye salmon flesh. The flow manifold was used to confirm the presence of astaxanthin in the crustacean samples. Also, an HPLC/UV-vis method was used to ascertain that this compound was the major carotenoid extracted under the optimum SFE conditions employed. The influence of SFE operating variables such as pressure, temperature, equilibration time, extraction time, trap temperature, and volume of CO₂ modifier was examined in order to maximize the efficiency of analyte extraction. The use of supercritical CO₂ enables the expeditious, selective, quantitative extraction of astaxanthin from crustaceans.     

Application of totally automated on-line sample clean up for prostanoid extraction and HPLC separation

Summary The aim of this study has been the evaluation of an automated system for on-line sample preparation using solid phase extraction and HPLC purification for the measurement of prostanoids in urine. We have established the optimum precolumn and column conditions for this analysis. The manual extraction —HPLC procedure furnishes lower recoveries and higher coefficients of variation than those obtained by the automated on-line procedure. The automated system has been applied to prostanoid analysis of human urine samples from subjects exposed to lead.     

On-line hyphenation of supercritical fluid extraction and two-dimensional high performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometer for the analysis of Ganoderma lucidum

A novel on-line system combining supercritical fluid extraction (SFE) and two-dimensional high performance liquid chromatography (2D-HPLC) was developed. A trap column and two three-port valves were employed to couple SFE and 2D-HPLC system, which was composed of a CN column and a monolithic silica column, connected by a 10-port dual-position valve. The analytes extracted by supercritical CO2 were completely transferred to the 2D-HPLC system. After separation in two orthogonal modes, the eluents were delivered to APCI-tandem-MS for identification of the samples. In this way, sample preparation, separation, detection, and identification were integrated into an on-line system permitting analysis of the fruiting bodies of Ganoderma lucidum, and at least 73 components in the extract were resolved with calculated peak capacity of up to 1643.     

Rapid narrow band elution for on-line SPE using a novel solvent plug injection technique

Determination of trace constituents in biological and environmental samples usually requires a pre-concentration step. While solid-phase extraction (SPE) has been widely used, it is slow, labor intensive and adversely affected by analytical errors from handling. On-line SPE eliminates some of the flaws but often suffers from solvent compatibility problems with the subsequent chromatography separation. In this study, we are presenting a technical solution for overcoming some of these compatibility issues, by utilizing a fully automated, focused SPE sample transfer technique utilizing narrow-band solvent plugs, for seamless hyphenation with high-performance liquid chromatography (HPLC) or flow injection mass spectrometry (MS). A wide range of pharmaceutical compounds was studied in different sample matrices. Short plugs of high elution strength solvent were generated by means of an electrically actuated sample loop and enrichment and transfer steps monitored using on-line SPE-MS. The impact of the solvent plugs on chromatographic separation was studied using hyphenated SPE-LC-MS. By carefully examining elution profiles of solvent plugs of different compositions, optimum conditions for quantitative elution within well-defined volumes were found for all substances. In addition, the highly focused elution bands resulted in excellent retention time and peak area reproducibilities when injected on-line onto HPLC columns. Finally, to demonstrate proof-of-principle, the fully integrated on-line SPE-LC-MS system was applied to the analysis of spiked urine and river water samples.     

Robotic solid phase extraction and high performance liquid chromatographic analysis of ranitidine in serum or plasma.

A fully automated assay for the analysis of ranitidine in serum and plasma, with and without an internal standard, was validated. It utilizes robotic solid phase extraction with on-line high performance liquid chromatographic (HPLC) analysis. The ruggedness of the assay was demonstrated over a three-year period. A Zymark Py Technology II robotic system was used for serial processing from initial aspiration of samples from original collection containers, to final direct injection onto the on-line HPLC system. Automated serial processing with on-line analysis provided uniform sample history and increased productivity by freeing the chemist to analyse data and perform other tasks. The solid phase extraction efficiency was 94% throughout the assay range of 10-250 ng/mL. The coefficients of variation for within- and between-day quality control samples ranged from 1 to 6% and 1 to 5%, respectively. Mean accuracy for between-day standards and quality control results ranged from 97 to 102% of the respective theoretical concentrations.     

Routine determination of benzo[a]pyrene at part-per-billion in complex industrial matrices by multidimensional liquid chromatography

A rapid and selective high performance liquid chromatography (HPLC) method using a column-switching technique has been developed for the determination of benzo[a]pyrene in complex mixtures containing polycyclic aromatic hydrocarbons. The diluted sample is directly injected into the chromatographic system without pre-treatment. The purification is performed on-line using three cleaning columns filled with various stationary phases. The sample preparation, a simple dilution, and the analysis time do not exceed 45 min. The method developed was used to analyze industrial products such as oil, bitumen, etc. and was compared with an off-line method requiring treatment and extraction steps before the analysis.     

On-line automated sample preparation for liquid chromatography using parallel supported liquid membrane extraction and microporous membrane liquid-liquid extraction

An automated system was developed for analysis of non-polar and polar ionisable compounds at trace levels in natural water. Sample work-up was performed in a flow system using two parallel membrane extraction units. This system was connected on-line to a reversed-phase HPLC system for final determination. One of the membrane units was used for supported liquid membrane (SLM) extraction, which is suitable for ionisable or permanently charged compounds. The other unit was used for microporous membrane liquid-liquid extraction (MMLLE) suitable for uncharged compounds. The fungicide thiophanate methyl and its polar metabolites carbendazim and 2-aminobenzimidazole were used as model compounds. The whole system was controlled by means of four syringe pumps. While extracting one part of the sample using the SLM technique. the extract from the MMLLE extraction was analysed and vice versa. This gave a total analysis time of 63 min for each sample resulting in a sample throughput of 22 samples per 24 h.     

Monitoring the Progress of a Photochemical Reaction Performed in Supercritical Fluid Carbon Dioxide Using a Continuously Stirred Reaction Cell Interfaced to On-Line SFC

A high-pressure photochemical reaction cell operated with a magnetic stir drive has been directly interfaced on-line with either SFC or HPLC. The interface consisted of an oven housing a recirculation pump directly connected to a sample injection valve. The inlet of the recirculation pump and the outlet from the sample injection valve were connected to the stirred reaction cell such that a return flow circuit was established. With this arrangement, a continuous flow of fresh supercritical fluid photochemical reaction mixture was maintained through the sample injection valve. This enabled samples of reaction mixture to be conveniently analyzed at regular intervals to monitor reaction progress using either on-line SFC or HPLC. The photoreduction of benzophenone in the presence of propan-2-ol to produce 1,1,2,2-tetraphenylethane-1,2-diol and 2-methyl-1,1-diphenylpropan-1,2-diol was studied. For this reaction, on-line SFC provided significantly better performance than on-line HPLC and was therefore used to monitor overall reaction progress and the different product yields. Quantitative results for this study demonstrate that highly efficient photochemical reactions proceeded in supercritical fluid carbon dioxide at 13 and 20 MPa.