A novel method for quality consistency evaluation of Glycyrrhiza formula granules based on a spectrum-effect study

Quality consistency of Glycyrrhiza formula granules is essential for guaranteeing clinical efficacy. However, a suitable method to accurately and conveniently evaluate the consistency of the clinical efficacy of Glycyrrhiza formula granules is currently not available. This study established a method for the simultaneous determination of 12 active components in Glycyrrhiza formula granules using ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight tandem mass spectrometry. The rate of inhibition of cyclooxygenase-2 by different batches of Glycyrrhiza formula granules was determined. Near-infrared spectra were collected for different batches of Glycyrrhiza formula granules to detect their biological activity in the inhibition of cyclooxygenase-2. The quality consistency of the 11 batches of Glycyrrhiza formula granules was evaluated using principal component and correlation analyses. The results showed significant differences in the formula granules of Glycyrrhiza uralensis produced by the different manufacturers. Some differences were also observed among batches of formula granules produced by the same manufacturer. Correlation analysis of the chemical components and cyclooxygenase-2 activity showed that glycyrrhizic acid, liquiritin, and isoliquiritin were the main active components of Glycyrrhiza. Correlation analysis of the near-infrared spectra and cyclooxygenase-2 inhibition activity showed a high correlation between the active components and three characteristic bands: 3383–3995, 4227–4651, and 5315–5878 cm⁻¹. In this study, the main active anti-inflammatory components of Glycyrrhiza granules were screened. Thus, the near-infrared spectrum and characteristic active band of multi-index active components can be used to quickly detect the quality consistency of Glycyrrhiza formula granules, thereby improving the ability to control the quality and consistency of these granules.     

色谱及相关技术在中药质量评价中的应用

对中药物质基础的研究方法——化学物质组学,以及中药质量评价的关键技术——指纹图谱技术做了介绍,并在此基础上综述了中药化学信息获取的关键技术——色谱及相关技术在中药质量评价中的应用。论述的结果表明,以化学物质组学为指导,结合色谱及相关技术获取指纹图谱信息及多指标成分定量信息的研究模式,对中药质量评价体系的建立具有指导意义。     

雄县地下水多组分含量分析及水质评价

为了解雄县地区地下水水化学特征及水质现状,选取43组地下水,采用仪器分析和容量法相结合的方式对雄县地下水典型的环境项目进行测定,运用数理统计和三元相图分析了雄县地下水的主要离子特征,并运用综合评价法对地下水质量予以评价。结果表明,该类指标的方法检出限为0.001～1.30mg/L,相对标准偏差为0.30%～3.7%,pH值和偏硅酸空间变异最低(CV30%),Mg~(2+)、Cl~-、SO_4~(2-)和碘化物的空间变异性最高(CV100%),水化学类型主要以HCO_3-Na型为主,水质评价结果显示研究区域地下水水质总体状况较好,多为Ⅱ类水和Ⅲ类水。研究成果对了解雄县地下水水质现状具有重要意义。     

Combination of the advantages of chromatographic methods based on active components for the quality evaluation of licorice

A rapid, improved and comprehensive method including high‐performance thin‐layer chromatography, fingerprint technology and single standard to determine multiple components was developed and validated for the quality evaluation of licorice. In this study, a newly developed high‐performance thin‐layer chromatography method was first used for authentication of licorice, which achieved simultaneous identification of multiple bands including five bands for known bioactive components by comparing their retention factor values and colors with the standards. For fingerprint analysis, 8 of 16 common peaks were identified. Simultaneously, similarity analysis which showed very similar patterns and hierarchical clustering analysis were performed to discriminate and classify the 27 batches of samples. Additionally, the single standard to determine multiple components method was first successfully achieved to quantify the eight important active markers in licorice including liquiritin apioside, liquiritin, isoliquiritin apioside, isoliquritin, neoisoliquiritin, liquiritigenin, isoliquiritigenin and glycyrrhizic acid. The easily available glycyrrhizic acid was selected as the reference substance to calculate relative response factors. Compared with the normal external standard method, this alternative method can be used to determine the multiple indices effectively and accurately. The validation result showed that the developed method was specific, accurate, precise, robust and reliable for the overall quality assessment of licorice.     

Application of thermogravimetry in the quality control of mebendazole

A study was made of the thermal behavior of the starting materials, their mixtures and the resulting mebendazole tablets. The thermal curves were obtained with a Shimadzu thermobalance, model TGA-50, using an air flow of 50 mL min^–1 and a heating rate of 10°C min^–1 in the temperature interval 30–900°C. The reaction constant velocities for the mebendazole salt and tablets were determined isothermally, using the Arrhenius expression. The thermal stability of mebendazole tablets is lower than that of the mebendazole salt, due to the presence of starch and lactose in the composition. Analysis of the data reveals that thermogravimetry is a powerful tool in pharmaceutical technology and quality control.The authors thank CNPq/PADCT for financial support.     

基于TPACK研究手持技术在中学化学课堂教学的应用现状

为了解中学化学教师对手持技术的应用水平和影响因素。以整合技术的学科教学知识（TPACK）理论为依据,创新性地将境脉（Context）因素引入TPACK调查中进行问卷设计,并对来自于全国16个省直辖市的187位教师进行了网络问卷调查,同时采用SPSS软件对问卷进行信效度评价,采用SPSS AMOS对问卷进行探索性因子分析,并对调查结果进行分析。研究结果显示中学化学教师手持技术TPACK量表结构模型较好,能够用于评价中学化学教师的手持技术应用水平;中学化学教师手持技术应用情况良好,但是与性别、教龄、学校类别有显著关系。针对研究结果,提出提高中学化学教师手持技术应用水平的发展建议,以期提高中学化学教师手持技术在中学化学教学的应用水平。     

In-house validation for analytical methods and quality control for risk evaluation of chlordecone in food

Chlordecone was used until 1993 as a pesticide in the banana plantation of Martinique and Guadeloupe (French Antilles) against the root borer. This organochlorine pesticide was lipophilic, remnant, and toxic for human beings with both acute and chronic effects. Chlordecone was strongly absorbed and stored in soil and weakly decomposed in environment. Surveys conducted in 2001 revealed its presence in soil, rivers, and domestic food products. Local food (fruits and vegetables, cattle, poultry, and fish) was growing on soils, widely contaminated by chlordecone, used in the past as banana plantations. In 2003, French Administration asked for a risk evaluation for the Antilles population. The French Agency for Food Safety, proposed a Provisional Tolerable Daily Intake of 0.0005?mg?kg^?1?b.w.?day^?1, and an Acute Reference Dose of 0.01?mg?kg^?1?b.w.?day^?1, based on a toxicological risk assessment. The French National Reference Laboratory for pesticides has carried out two analytical methods, one for food of animal origin and another for food of fruit and vegetable origin. These methods were validated in the reference laboratory and dispatched to 13 laboratories for a proficiency test before the launch of two studies on Martinique and Guadeloupe food. About 900 samples from Martinique were sent to the network of laboratories for analysis of chlordecone. Performance parameters obtained through the proficiency test were briefly reported. The quality control test proposed in this study was discussed to shed light on the true variability achievable by intra-laboratory and inter-laboratory analysis. The limits of conventional quality-control procedures were discussed, and a process was proposed in order to get better confidence in analytical results.     

咪唑类离子液体的合成及其在分析化学中的应用

本文介绍了咪唑类离子液体的合成,特别是以BF4-、PF6-为阴离子的咪唑类离子液体的合成,并重点综述了近年来咪唑类离子液体在电化学分析、质谱、光谱、色谱及毛细管电泳等分析化学中的应用.     

Future trends in analytical quality assurance — the estimation of uncertainty

This paper presents one of the future trends in analytical quality assurance, the evaluation of the quality of analytical results by estimation of their uncertainties. The present state-of-the-art is described, and the impact caused by the declaration of uncertainties in chemical results is foreseen.     

美国Journal of Chemical Education中信息技术在化学教学中运用的文献分析

从年份和内容分类分析了2012-2018年Journal of Chemical Education中信息技术在化学教学中的运用研究发文情况,介绍了4篇具有代表价值的主推实例,总结了当前国际化学教育研究现状与趋势。     

Recent analytical approaches in quality control of traditional Chinese medicines—A review

Traditional Chinese medicines (TCMs) are gaining more and more attention all over the world, due to their specific theory and long historical clinical practice. But the uncontrollable quality is a bottleneck for its modernization and globalization. This paper reviewed the recent analytical methods in the quality control of TCMs, including screening strategies of bioactive markers from TCMs through biochromatographic methods, the traditional chromatographic methods, DNA methods, as well as the spectroscopic methods, including FT-IR, NIR and NMR. The comprehensive methods, such as fingerprint and multi-component quantification are emphasized; hyphenated techniques, like HPLC-MS, GC-MS, CE-MS, LC-NMR, chemometric methods, and combination of chemical and biological methods, such as biofingerprint, metabolic fingerprint are now more and more widely used in TCMs. In a few word, the analysis and quality control of TCMs are moving towards an integrative and comprehensive direction, in order to better address the inherent holistic nature of TCMs.     

The teaching potential of evaluation and optimization methods in analytical chemistry

Summary The teaching potential for analytical chemistry of some mathematical and statistical tools is discussed. It is concluded that some of the so-called chemometric techniques should be taught and that they permit to develop a philosophy of problem solving in analytical chemistry.

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Unterrichtsmöglichkeiten für Bewertungs- und Optimierungsmethoden in der Analytischen Chemie

Zusammenfassung Die Notwendigkeit der Aufnahme solcher Methoden in die Unterrichtspläne für Analytische Chemie wird diskutiert und eine Reihe von statistischen und mathematischen Verfahren (sog. Chemometrie) wird beschrieben, die sich für die Aufnahme in die Lehrpläne eignen.

     

A comparison in the evaluation of measurement uncertainty in analytical chemistry testing between the use of quality control data and a regression analysis

The evaluation of measurement uncertainties has been widely applied to the calibration of measurement instruments, whereas its application to tests, despite increasing requirements, is a more recent phenomenon. The generalization of the evaluation of measurement uncertainties to tests has been a gradual process, in line with changes in the requirements of the normative framework that regulates the accreditation of tests laboratories and also as the perceived good practices have evolved. The sole identification of the relevant sources of uncertainty was followed by the requirement to provide a simplified estimate of the measurement uncertainty, and it is now an accepted requirement to properly evaluate the expanded measurement uncertainty associated with any tests. In this study, the evaluation of measurement uncertainty associated with the determination of sulfate in water will be attempted using a procedure that includes linear regression, with the regression parameters provided with associated uncertainties, and a Monte Carlo method applied as a validation tool of the conventional mainstream evaluation method, concerning the approximations in terms of linearization of the model and the assumed shape of the output distribution introduced by this approach.     

分子印迹技术在药学中的应用进展

综述了分子印迹技术在手性药物分离、临床药物分析、药物传递系统、中药活性成分的分离纯化、药物残留检测中的应用,并对其面临的问题及应用前景进行了展望。     

“点击”反应在制备环状聚合物中的应用

环状聚合物具有不同于线性高分子的独特性质,是一类具有应用前景的新型聚合物材料,但复杂的结构导致其合成过程复杂繁琐.＂点击＂化学由于其高效、可靠、高选择性的特点已成为拓扑高分子合成的新方法,活性自由基聚合（ATRP、RAFT和NMP）具有聚合物结构可控等特点,二者联用为环状聚合物的合成拓宽了思路.本文就近几年＂点击＂反应、＂点击＂反应与活性自由基聚合联用以及其他方法联用在环状聚合物中的应用进行综述.＂点击＂反应与这些方法的结合将在功能性环状聚合物的设计与合成中发挥积极的作用.     

有色金属冶炼中含砷物料的除砷技术研究现状

综述了砷对冶金、环境以及人类的危害,阐述了冶金工业中含砷物料的除砷技术的发展现状,介绍了各种技术的原理、应用,分析了各种技术的优缺点,展望了除砷技术的发展方向。     

有色金属冶炼中含砷物料的除砷技术研究现状

综述了砷对冶金、环境以及人类的危害,阐述了冶金工业中含砷物料的除砷技术的发展现状,介绍了各种技术的原理、应用,分析了各种技术的优缺点,展望了除砷技术的发展方向。     

The teaching of analytical chemistry in the laboratory

Summary The operation of a combined inorganic analytical course designed to be as flexible as possible, and to use the student's time most economically is described. It has been found that students can be interested by carrying out experiments on their own preparations, but that considerable caution is needed in the interpretation of the results because their preparations may vary considerably and in a manner which is not predictable. The advantages and disadvantages of such a course are discussed.

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Analytisch-chemischer Unterricht im Laboratorium

Zusammenfassung Ein kombinierter anorganisch-analytischer Lehrgang wird beschrieben, der möglichst flexibel ist und die aufgewendete Zeit nutzbringend einzusetzen erlaubt. Durch Versuche mit eigenen Präparaten wird das Interesse des Studenten geweckt; jedoch ist bei der Auswertung der Ergebnisse Vorsicht geboten, da die Präparate unterschiedliche Zusammensetzung aufweisen können. Vor- und Nachteile eines solchen Lehrganges werden diskutiert.

Lecture presented at Euroanalysis I Conference, 28. 8.–1. 9. 1972 in Heidelberg, Germany.     

Synthesis of titania and titanate nanomaterials and their application in environmental analytical chemistry

TiO₂ nanoparticles and H₂Ti₂O₅·H₂O, Na₂Ti₂O₄(OH)₂ nanotubes were synthesized by solvothermal method and their applications in the degradation of active Brilliant-blue (KN-R) solution were investigated. The experimental results revealed that the synthesized TiO₂ nanoparticles had a good crystallinity and a narrow size distribution (about 4–5 nm); the obtained H₂Ti₂O₅·H₂O, Na₂Ti₂O₄(OH)₂ were tubelike products with an average diameter of 20–30 and 200–300 nm length. The three catalysts we synthesized had some hydroxyl groups and the maximum absorption boundaries of the samples were all red-shifted, which indicated the samples had a promising prospect in photocatalysis.

The results of the photocatalytic experiments indicated that the photocatalytic activity of the samples was: TiO₂ > H₂Ti₂O₅·H₂O > Na₂Ti₂O₄(OH)₂, which was in good accordance with the fact of FTIR and UV–vis absorption spectra. The formation mechanism of these nanostructures was also discussed.     

Quality management in analytical R&D in the pharmaceutical industry: Building quality from GLP

 The pharmaceutical industry is one of the most regulated activity sectors. The regulation includes specific quality systems such as good laboratory practice (GLP), good clinical practice (GCP) and good manufacture practice (GMP). The principles of GLP mainly cover the formal quality aspects of a procedure and do not evaluate the technical aspects in depth. On the other hand, EN 45001 accreditation covers technical performance and is not suitable for pharmaceutical research and development (R&D) as it is almost impossible to comply with the requirements of the European standard in the pharmaceutical environment. The challenge to the pharmaceutical industry is, therefore, to develop quality systems, compatible with GLP principles, that not only cover formal quality items but also ensure good scientific and technical performance. An implementation process focused on real quality improvement is the best way to achieve this objective, culminating in formal recognition of the quality system by third-party assessment. In the case of analytical R&D, the EURACHEM/CITAC Guide CG2 is a very good tool that can help in the definition, analysis and selection of the non GLP quality elements that will be useful. Received: 30 June 1999 / Accepted: 18 October 1999