色谱指纹图谱与中药质量控制

本文综述了近年来色谱指纹图谱研究中多种色谱技术、相关化学计量学方法的发展及其在中药质量控制中的应用,并对中药质量稳定性和有效性的全面评价方法和可行性进行了初步探讨。提出以色谱指纹图谱为核心,依托现代色谱技术、化学计量学和系统生物学方法,建立中药化学成分信息与药效(毒性)信息相关关系的中药质量控制研究策略,深层次揭示中药的内在作用机理,期望真正实现中药质量的可控、安全和有效。     

中药指纹图谱技术

介绍中药指纹图谱的研究内容、意义和特点 ,以及中药指纹图谱采集和信息处理的主要技术手段     

Qualitative and quantitative analysis in quality control of traditional Chinese medicines

Separation techniques with high efficiency and sensitive detection have been widely used for quality control of traditional Chinese medicines (TCMs). High-performance liquid chromatography, gas chromatography, and capillary electrophoresis are commonly used to separate various components in TCMs. Ultraviolet detection, fluorescence detection, evaporative light-scattering detection, mass spectrometry and nuclear magnetic resonance can be applied to separation techniques for qualitative and quantitative analysis of TCMs. The development of quality control for TCMs based on quantitative and qualitative analysis from 2000 to 2007 are reviewed; the fingerprint technique is also discussed due to its broad application in the quality control of TCMs. Prospects for further research based on our primary results are also discussed.     

中药质量控制技术发展展望

本文从中药产业需求、现代化需求、技术需求、机遇与挑战等方面概括了中药质量控制技术发展的背景;讨论了中药质量控制技术对于提高中药药效和安全性、推动产业发展和推进中药国际化的意义;综述了中药质量控制技术的现状,分析了在过程控制、安全性控制、标准品和对照品制备、指纹图谱技术等方面的不足;提出了中药质量控制技术应重点发展以分离和表征技术为主的中药质量控制关键技术、中药安全性控制技术、中药质量控制标准体系、中药质量控制原创性技术和中药标准品、对照品生产技术,制定技术标准,建立具有中药特色的过程控制和产品质量控制标准。     

A proficiency test scheme for the quality control of black tea and development of quality control material for internal quality control

A proficiency test (PT) was organized for quality control analysis of black tea. Test materials for the analyses of total content of powder tea, moisture, total ash, acid-insoluble ash, water-soluble ash, alkalinity of water-soluble ash, water extract, crude fiber and caffeine were sent to the participant laboratories (n:43) in 2009. The assigned value, standard deviation of the parameters and z-scores of the participant laboratories were calculated using the data reported by the participants. The percentage of the reported results for analytes was found to be ranged from 67.5 to 100%. Acceptable z-scores were achieved by 80.5–97.5% of the participant laboratories. More than 15% of unacceptable results were obtained for acid-insoluble ash and caffeine analyses. The quality control material for quality control analysis of black tea was developed from the remaining material.     

基于定量指纹图谱技术的中药质量控制

定量指纹图谱技术是中药指纹图谱技术与多指标成分定量分析相结合的中药质量控制模式。定量指纹图谱技术的发展包括定量组分的制备、过程控制的指纹图谱技术和产品含量测定3个主要部分。本文以丹参为例,通过水提、醇沉、过膜、大孔树脂分离和工业色谱分离5个工艺流程制备了丹参定量组分,对各个工艺步骤以指纹图谱技术考察其稳定性和重复性。对丹参定量组分中的原儿茶醛、迷迭香酸、丹酚酸B 3个成分进行含量测定。3个成分的含量总和大于50%。定量组分的制备以现有的活性成分为目标,经过去粗存精的工艺过程,其质量标准得到了有效的提高。     

Chromatographic fingerprinting and related chemometric techniques for quality control of traditional Chinese medicines

Development of chromatographic fingerprint (CF) and related chemometric methods and their applications to quality control of traditional Chinese medicines (TCMs) were discussed. CF is essentially a kind of quality control method for TCMs (or Chinese herbal medicines). Also, it is a quality‐relevant‐data high‐throughput and integral tool to explore chemically the complexity of TCMs. With the help of chemometrics, some difficulties in evaluation and analysis of CFs, such as calculation of information content, peak alignment, pattern analysis, deconvolution of overlapping peaks, etc. could be well solved. To further explore TCMs synergic quality, intensive study of CF coupled with chemometrics will create the possibility to achieve the aim to reveal the working mechanisms of TCMs and to further control and strengthen TCMs' intrinsic quality in a comprehensive manner.     

Understanding the traditional aspect of Chinese medicine in order to achieve meaningful quality control of Chinese materia medica

Although sophisticated and technologically advanced, current quality control methods for Chinese medicines (syn. Chinese materia medica or CMM) lack comprehensiveness and practicability. They are more suited for analyzing single-chemical drugs or specific, known chemical components that have already been isolated. While these methods can fully satisfy the modern scientific requirements for identity, purity and quality in the assessment of chemical drugs, they are not suitable for handling the complex chemical nature of traditional CMM whose multifunctional components along with their inherent holistic activities are frequently unknown and thus are not adequately analyzed by these methods. In order to assess properly and meaningfully the identity and quality of complex CMM (also known as Chinese herbs and Chinese herbal medicines), additional measures that can retain the traditional aspect of CMM need to be included. This requires a basic understanding of traditional Chinese medicine (TCM).     

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.     

Implementation of quality assurance system to enhance reliability in Chinese handwriting examination

In regard to the tightened standard on the acceptance of forensic evidence at courts, in particular the evidence-based opinion, the forensic community worldwide is striving to improve test reliability through the implementation of quality assurance system. Handwriting examination including Chinese handwriting is a typical traditional forensic discipline that has often been subjected to judicial challenges in courts. In this paper, we present the work practice and the quality control procedure for Chinese handwriting examination in accordance with ISO/IEC 17025, an international standard on general requirements for the competence of testing and calibration laboratories. The examination work constitutes various phases of identification of the characteristic writing features, comparison and evaluation of the significant similarities and differences, interpretation of findings and formation of opinions. With the support of a fit-for-the-purpose quality system complying with the ISO standard, document examiners in this laboratory are obliged to address the criteria as stated in the pre-set quality assurance plan and undertake scrupulous efforts in delivering the scientific work at all stages throughout their examinations. By doing so, personal bias and other subjective factors that cause detrimental influence to the formation of expert opinions would be kept to a minimum.     

Tentative fingerprint-efficacy study of Houttuynia cordata injection in quality control of traditional Chinese medicine

To establish potent fingerprint for quality control of traditional Chinese medicine, Houttuynia cordata (Saururaceae) injection (HCI), the attempt on fingerprint-efficacy was developed in this study. HCI from ten different factories were determined by gas chromatography-mass spectrum (GC-MS) and classified by hierarchical clustering. The anti-inflammatory effect of HCI was characterized with the rat pleurisy model induced by carrageenin and the mice ear edema model by xylene. The results showed that anti-inflammatory effect of the injections from most of factories on the two models was significant. There was corresponding relationship between the fingerprint of HCI and efficacy to certain extent. The main common constitutes in injection from the factories that possess anti-inflammatory activity were analysed with GC-MS and identified using the NIST Mass Spectral Database. This common pattern of HCI based on the efficacy was helpful for the purpose of quality control.     

Plans for implementation of a quality system in the control laboratory of the Romanian National Medicines Agency

This paper describes the practical implementation of a quality system in the control laboratory of the National Medicines Agency, Romania, the main aim being the alignment of the requirements of the control of drugs in Romania with European Union standards. Activity in this field is relatively new in Romania, however, it is of great importance to Romania’s compliance with international standards. Received: 13 September 2000 Accepted: 19 February 2001     

Development of a new certified reference material of high-purity chrysin for the quality control of traditional Chinese medicine

Chrysin, a naturally occurring flavone, extracted from traditional Chinese herbs and abundantly found in propolis has been known to exhibit a wide range of biological activities, such as antioxidant, anti-inflammatory, hypolipidemic, anti-hypertensive, anti-diabetic, and anti-tumour activities. Among this, its anticancer effects make chrysin promising to be a candidate drug. The objective of this study was to develop a new certified reference material (CRM) for the quality control of traditional Chinese medicine, chrysin, and the related pharmaceuticals. The studies of sample preparation, homogeneity, stability, value assignment, and uncertainty evaluation were accomplished in this paper. Two different methods, namely differential scanning calorimetry and coulometric titration, were utilized for the first time to determine the purity of chrysin. The purity of the high-purity chrysin CRM, after validation and evaluation, was certified to be (0.996 ± 0.015) g/g (k = 2).     

安尔眠糖浆剂型改良与质量控制

本文建立了安尔眠糖浆剂型改良成丸剂的制备工艺及其含量测定的方法。结果表明,制备工艺稳定、可行。用HPLC法测定安尔眠丸的含量,在0.25～1.23μg范围内,线性关系良好,平均加样回收率为99.68%,RSD为1.33%。该测定方法简便,结果可靠,重现性好,可作为安尔眠丸的含量测定方法。     

Advanced automation of a flow injection analysis system for quality control of olive oil through the use of a distributed expert system

A new methodology—based on the combination of flow injection analysis and a distributed expert system—is proposed for the on-line chemical quality control of olive oil. This knowledge-based system is in charge of carrying out the flow injection determination of total acidity, peroxide value, and UV spectrophotometric measurements (K₂₃₂ and K₂₇₀), according to EU legislation. On the other hand, the expert system, apart from supervising the correct functioning of the system (devices, clogging, analysis frequency, and so on), performs the definite classification of the analyzed oil by evaluating the oil quality from the values yielded, according to previously established specifications. Satisfactory results have been obtained in the application of this approach to different samples of Spanish olive oil along the storage process. The distributed expert system also allows for the remote control of the analysis process owing to the interconnection of the different nodes by means of a communication network.     

Uncertainty-based measurement quality control

According to a simple acceptance decision rule for measurement quality control, a measured value will be accepted if the expanded uncertainty of the measurements is not greater than a preset maximum permissible uncertainty. Otherwise, the measured value will be rejected. The expanded uncertainty may be calculated as the z-based uncertainty (the half-width of the z-interval) when the measurement population standard deviation σ is known or the sample size is large (30 or greater), or by a sample-based uncertainty estimator when σ is unknown and the sample size is small. The decision made based on the z-based uncertainty will be deterministic and may be assumed to be correct. However, the decision made based on a sample-based uncertainty estimator will be uncertain. This paper develops the mathematical formulations for computing the probability of acceptance for two sample-based uncertainty estimators: the t-based uncertainty (the half-width of the t-interval) and an unbiased uncertainty estimator. The risk of incorrect decision-making, in terms of the false acceptance probability and false rejection probability, is derived from the probability of acceptance. The theoretical analyses indicate that the t-based uncertainty may result in significantly high false rejection probability when the sample size is very small (especially for samples of size 2). For some applications, the unbiased uncertainty estimator may be superior to the t-based uncertainty for measurement quality control. Several examples from acoustic Doppler current profiler streamflow measurements are presented to demonstrate the performance of the t-based uncertainty and the unbiased uncertainty estimator.