High‐resolution mass spectrometry for bioanalytical applications: Is this the new gold standard?

Liquid chromatography coupled to quadrupole‐based tandem mass spectrometry (QqQ) is termed the “gold standard” for bioanalytical applications because of its unpreceded selectivity, sensitivity, and the ruggedness of the technology. More recently, however, high‐resolution mass spectrometry (HRMS) has become increasingly popular for bioanalytical applications. Nonetheless, this technique is still viewed, either as a screening technology or as a research tool. Although HRMS is actively discussed during scientific conferences, it is yet to be widely utilised in routine laboratory settings and there remains a reluctance to use HRMS for quantitative measurements in regulated environments. This paper does not aim to comprehensively describe the potential of the latest HRMS technology, but rather, it focuses on what results can be obtained and outlines the author's experiences over a period of many years of the routine application of various forms of HRMS instrumentation. Fifteen years ago, some nine different QqQ methods were used in the author's laboratory to analyse a variety of different veterinary drug resides. Today, many more analytes are quantified by seven HRMS methods and just three QqQ methods remain in use for the analysis of a small set of compounds yet to be upgraded to HRMS analysis. This continual upgrading and migration of analytical methods were accompanied by regularly participating in laboratory proficiency tests (PTs). The PT reports (covering a range of analytes and analytical methods) were used to compare the accuracy of HRMS‐ versus QqQ‐based measurements. In the second part of this paper, the particular strengths and limitations of HRMS for both method development and routine measurements are critically discussed. This also includes some anecdotal experiences encountered when replacing QqQ assays with HRMS methods.     

ORCADIAN OSCILLATORS AND PHOTORECEPTORS IN THE GASTROPOD,APLYSIA*

Abstract— The sea slug, Aplysia, is a useful model system for research on the neurophysiology of circadian integration. The animal contains several circadian oscillators and several photoreceptors. Each eye contains a circadian oscillator as well as photoreceptors. The ocular oscillators can be entrained by extraocular photoreceptors as well as their own ocular photoreceptors. The abdominal ganglion probably contains another oscillator but it has been much more difficult to manipulate in the laboratory than have the oscillators in the eyes. There is also a circadian rhythm in overt behavioral activity. This rhythm is controlled in part by extraocular oscillators and extraocular photoreceptors and in part by the eyes. In exerting their influence on the behavioral rhythm, the eyes appear to act in the capacity of oscillators and not merely as photoreceptors. Although neurons in the retina have neurosecretory morphology, the entire influence of the eyes on the behavioral rhythm appears to be mediated by nerve signals which travel in the optic nerve. As yet there is no evidence to suggest that any two oscillators in Aplysia are internally coupled. There is also no evidence yet for hormonal coupling between photoreceptors and oscillators or between oscillators and rhythmic outputs.     

ON THE CHROMOPHORE CONFIGURATION OF METARHODOPSIN II

Abstract The nature of the chromophore configuration of metarhodopsin II (meta II) has been a subject of recent controversy. Earlier resonance Raman results from this laboratory had indicated that meta II has an unprotonated Schiff base linkage between the chromophore and apoprotein. It has been argued, on the other hand, that the Raman evidence does not exclude a non-covalently bound retinal chromophore. In this communication we present additional evidence and further arguments in favor of our earlier conclusion regarding the state of the chromophore in meta II.     

DETERMINATION OF THE DEGREE OF BONDED PHASE ON THE SURFACE OF SILICA GEL BY XPS

Attention is being increasingly paid to the new material prepared by bonding organic molecules on the surface of silica gel in the preparation of catalyst or packing material for liquid chrotnatographic column.There has not been a quantitative method for determination or characterizing the degree of bonded phase on surface of silica gel yet.This paper provides a new semi-quantitative method.     

浅析化学生物学实验课程的有效教学方法

作为高年级化学专业本科生的综合性实验课程,化学生物学实验课为学生提供了拓宽知识体系及培养相关实验技术能力的平台。本文主要介绍了笔者在改进实验课教学过程中所做的尝试,包括设置"实验考查点"以提高实验效率,通过"翻转课堂"形式引入改进内容以及根据教材合理拓宽实验内容等。多种方式的综合应用有助于教与学的互动,更适应实验课程交叉性和不断发展的需要。     

Tinkering with Mechanochemical Tools for Scale Up

Mechanochemistry provides an environmentally benign platform to develop more sustainable chemical processes by limiting raw materials, energy use, and waste generation while using physically smaller equipment. A continuously growing research community has steadily showcased examples of beneficial mechanochemistry applications at both the laboratory and the preparative scale. In contrast to solution-based chemistry, mechanochemical processes have not yet been standardized, and thus scaling up is still a nascent discipline. The purpose of this Minireview is to highlight similarities, differences and challenges of the various approaches that have been successfully applied for a range of chemical applications at various scales. We hope to provide a discussion starting point for those interested in further developing mechanochemical processes for commercial use and/or industrialisation.     

探索战略性新兴产业发展模式,推动纳米技术应用产业发展

作为开展纳米科技研究较早、论文专利成果显著的纳米科技大国,我国的纳米技术产业化发展明显滞后,尚未形成纳米技术的＂产业＂共识.苏州是国内第一个把纳米技术产业作为引领转型升级的战略性新兴产业的区域,这一战略选择得到了国家、中国科学院和江苏省的高度支持.战略性新兴产业发展需要＂顶层设计、系统规划＂.苏州借鉴国际经验,结合国情和区域实际,提出构建纳米技术产业生态圈,按照产业发展需求规划布局和整合产业资源要素,形成有效互动的产业发展模式,得到国内外纳米技术科技界、产业界和政府部门的普遍认同.     

Capillary electrophoresis and the clinical laboratory

Over the past 15 years, CE as an analytical tool has shown great promise in replacing many conventional clinical laboratory methods, such as electrophoresis and HPLC. CE's appeal was that it was fast, used very small amounts of sample and reagents, was extremely versatile, and was able to separate large and small analytes, whether neutral or charged. Because of this versatility, numerous methods have been developed for analytes that are of clinical interest. Other than molecular diagnostic and forensic laboratories CE has not been able to make a major impact in the United States. In contrast, in Europe and Japan an increasing number of clinical laboratories are using CE. Now that automated multicapillary instruments are commercially available along with cost-effective test kits, CE may yet be accepted as an instrument that will be routinely used in the clinical laboratories. This review will focus on areas where CE has the potential to have the greatest impact on the clinical laboratory. These include analyses of proteins found in serum and urine, hemoglobin (A1c and variants), carbohydrate-deficient transferrin, forensic and therapeutic drug screening, and molecular diagnostics.     

STORM DEPOSITS IN THE CHANGJIANG DELTA

Based on over 10 years' field survey and laboratory work, it has been confirmed that a series of storm deposits have been developed on different geomorphological and sedimentological zones in the Changjiang Delta, covering marsh lowland, shelly and sandy cheniers, tidal flats, the delta front and prodelta. The storm deposit model of the Changjiang Delta is particularly characterized by the hummocky cross stratification found above the normal wave base.     

焦磷酸盐溶液中铜电沉积过程 Ⅱ. 用旋转电极的研究

焦磷酸铜络合物还原过程中要经过一价铜这个中间产物在一些文献中都假设过。这个问题不仅是有兴趣的理论问题,而且也很有实际价值。因为在工业电镀中经常出现的所谓“铜粉”,常常影响镀层的质量。简单的Cu~(2+)离子在氧化物溶液中进行阴极还原时,曾经用旋转圆环-圆盘电极(RRDE)的方法实验证实了一价铜中间产物的存在。但是在铜以络离子存在时,尤其是在过剩的焦磷酸离子存在下,使得还原在较负的电位下进行。这时是否有一价铜中间产物,尚未见到RRDE的研究。用RRDE研究络离子还原的工作还很少。可是这一有力方法的应用将会揭示许多一般方     

以举办化学实验竞赛为契机,推动化学实验教学发展

第10届大学生化学实验竞赛在北京化工大学成功举行,大学生化学实验竞赛能检验学生掌握化学实验技能和操作水平的情况,促进学生更好地了解和掌握实验仪器,锻炼学生的动手能力和创新意识,培养学生严谨科学的态度。通过"北京市大学生化学实验竞赛"这个平台,高校之间更好地交流了化学实验教学的经验,并以此为契机促进化学实验教学的改革,提高化学实验教学水平。     

Protein fold recognition

Summary An important, yet seemingly unattainable, goal in structural molecular biology is to be able to predict the native three-dimensional structure of a protein entirely from its amino acid sequence. Prediction methods based on rigorous energy calculations have not yet been successful, and best results have been obtained from homology modelling and statistical secondary structure prediction. Homology modelling is limited to cases where significant sequence similarity is shared between a protein of known structure and the unknown. Secondary structure prediction methods are not only unreliable, but also do not offer any obvious route to the full tertiary structure. Recently, methods have been developed whereby entire protein folds are recognized from sequence, even where little or no sequence similarity is shared between the proteins under consideration. In this paper we review the current methods, including our own, and in particular offer a historical background to their development. In addition, we also discuss the future of these methods and outline the developments under investigation in our laboratory.     

Electrochemical treatment of tumours

The electrochemical treatment (EChT) of tumours implies that tumour tissue is treated with a continuous direct current through two or more electrodes placed in or near the tumour. The treatment offers considerable promise of a safe, simple and relatively noninvasive anti-tumour therapy for treatment of localised malignant as well as benign tumours. Although more than 10,000 patients have been treated in China during the past 10 years, EChT has not yet been universally accepted. The reason for this is the lack of essential preclinical studies and controlled clinical trials. Uncertainties regarding the destruction mechanism of EChT also hinder the development of an optimised and reliable dose-planning methodology. This article reviews the collected Chinese and occidental experiences of the electrochemical treatment of tumours, alone and in combination with other therapies. The current knowledge of the destruction mechanism underlying EChT is presented along with different approaches towards a dose planning methodology. In addition, we discuss our view of different important parameters that have to be accounted for, if clinical trials are to be initiated outside of China.     

X-光电子能谱仪的管理与维护

X-射线光电子能谱仪(XPS)是表面分析领域的重要工具,其快速发展促进了表面化学领域研究的深入.正确的使用和良好的维护不仅可以确保XPS始终保持良好的运行状态,还可以延长它的使用寿命.结合作者在实验室的工作经验和体会,从测试和维护仪器等方面介绍了管理和维护的经验,为相关人员提供参考.     

交联聚N-(乙烯苄基)乙二胺的合成(Ⅰ)

聚N-(乙烯苄基)乙二胺是一种很有用的功能基高聚物。但在直接胺化的合成过程中,乙二胺的两端反应极易发生,常导致严重的附加交联,因而产物中的伯胺基含量大大降低。通过对直接胺化反应的改进,乙二胺的两端反应可控制在较小的比例,从而提高了伯胺基的含量。在另一方法中,乙二胺的一个胺基先被酰化保护起来,这样在胺化时就避免了乙二胺的两端反应。在随后的水解过程中,伯胺基又被释出。上述两种方法制得的产物均接近我们所要合成的结构。它们的链霉素吸附试验结果,显示了预期的效果。     

THE LITHIUM CHLORIDE/DIMETHYLACETAMIDE SOLVENT FOR CELLULOSE: A LITERATURE REVIEW

Abstract

Cellulose or poly(1·4)-β-D-D-glucose is the most abundant, renewable organic raw material [1]. The molocular structure (Fig. 1) consists of cellobiose repeating units which allow chain-packing by intermolecular [2] and intramolecular [3] hydrogen-bonding. Such strong interactions are responsible for excellent inherent mechanical properties, yet at the same time, interfere with efforts to process or modify the material. Only in a few instances have cellulose derivatives been exploited commercially and certainly not to the extent predicted from raw material availability and cost. Controllable, uniform derivatization has been hampered by the lack of suitable, nondegrading solvents or by a limited range of synthetic reactions within these solvents.     

Assessors’ attitudes toward and experiences of national quality standards: a qualitative study in Iran

To establish a national accreditation system for medical laboratories, Iran has set national standards based on the international standard ISO 15189. Central to the accreditation process are the technical assessors. Their attitude in this regard and their experiences should be identified. This study aims to explore assessors’ attitudes toward national laboratory accreditation and their experiences of assessment process in order to identify current gaps and suggest required interventions to solve them. A qualitative study using an open-ended questionnaire was employed. A total of 150 assessors working in the General Directorate of Laboratory Affairs participated in the study. While almost all Iranian laboratory accreditation assessors were generally supportive about the necessity of laboratory accreditation and cited benefits of this process, they pointed to improvement areas including developing assessor selection and appraisal criteria, continuous training, taking into consideration the heterogeneity of laboratories throughout the country, participation of professional associations and adopting measures to increase laboratories’ involvement.     

Student-Designed Multistep Synthesis Projects in Organic Chemistry

The incorporation of research projects into undergraduate chemistry courses provides a perspective that is fundamentally unavailable in most laboratory experiences. While independent, multistep synthesis projects in organic chemistry have been reported previously, most efforts have been directed at relatively restricted, closely guided research plans with modest student participation in the experimental design. We have implemented a more open-ended synthesis project, limited principally by cost, safety and availability of materials. In the second semester of the sophomore organic sequence, students develop multiple drafts of a plan for a three-to-four-step synthesis. Subsequently, students obtain their own literature protocols for the individual steps. The synthesis is performed over three four-hour laboratory periods. The students conclude this project with a poster presentation of the results at the end of the semester. Evaluation of the students work focuses not only on the successful synthesis of the target but also on planning, troubleshooting, purification, and spectral analysis.     

中日合作废气处理项目分析实验室管理的几点经验

为顺利开展中日合作废气处理项目，中国石油化工股份有限公司环境监测总站建立了废气分析实验室，并完善了质量控制、质量保证体系，这些管理体系包括实验室物资设备的管理，实验室环境，质量保证体系，废气样品采集及实验室分析手段等。为废气处理项目的实施提供了有力的技术支持，并实现了实验室管理的科学化、标准化、规范化。