微波消解ICP-MS法测定海藻羊栖菜中多种有害元素

目的对海藻羊栖菜中的砷、镉、汞、铅、钴、镍、钒等多种有害元素进行分析。方法使用微波消解ICP-MS法同时检测上述多种有害元素,并对所建立的方法进行了方法学验证。结果结果表明羊栖菜中砷和镍的污染程度较高,同时探讨了有害成分的限量标准。结论该方法为海藻羊栖菜的风险监控提供了技术参数。     

基于特征甾醇谱的中药海藻鉴别研究

目的 基于指纹图谱和化学模式识别法开展中药海藻的鉴别研究。方法 收集多批次羊栖菜及同属常见混淆品,GC-MS法靶向建立植物甾醇指纹谱；运用主成分分析、正交偏最小二乘判别分析等化学模式识别方法,比较羊栖菜与混淆品的甾醇指纹谱差异,依据变量投影重要性数值筛选可用于中药鉴别的标志物。结果 建立了马尾藻植物甾醇指纹谱,精密度、重复性、稳定性良好；标定13个共有甾醇,利用对照品及NIST数据库鉴定了其中10个；以化合物摩尔比为变量,采用化学模式识别法能够明显区分羊栖菜与同属伪品,发现岩藻甾醇、马尾藻甾醇和24-酮基胆固醇这三者的含量之和可用于羊栖菜鉴别。结论 本研究建立了基于植物甾醇谱的化学判别模型,能够区分羊栖菜与同属混淆品,并为中药海藻(羊栖菜)鉴别提供候选质量标志物。     

羊栖菜多糖抗肿瘤作用的研究进展

目的:对国内外羊栖菜多糖(SFPS)抗肿瘤作用研究以及羊栖菜多糖抗肿瘤机制的研究进展进行综述。方法:查阅近期有关羊栖菜多糖抗肿瘤研究的相关文献,进行分类,归纳,整理与分析。结果:羊栖菜多糖抗肿瘤研究目前已有较多报道,并且取得了一定的成绩。结论:羊栖菜多糖抗肿瘤作用及其机理的研究已进行的较为深入。随着科学的进步对其抗肿瘤机制也有了新的认识。     

7种马尾藻属海藻碘及微量元素的含量测定

采用紫外－可见分光光度法测定了７种马尾藻属海藻羊栖菜，海蒿子、海子，鼠尾藻，铜藻，匐枝马尾藻和半叶马尾藻碘含量，采用原子吸收分光光度法测定了常量元素铁，钙和微量元素锌，铜，铅，镉等的含量。     

气相色谱-串联质谱法测定海藻羊栖菜中的19种有机氯农残

摘 要 目的：建立海藻羊栖菜中19种有机氯农药残留分析的气相 质谱联用方法。方法: 使用GC MS法同时检测19种农药残留,色谱系统采用HP 5MS毛细管色谱柱（30 m×0.25 mm,0.25 μm）;柱温为程序升温,初始温度70℃,保持1 min,以15℃·min^-1 升温至180℃,再4℃·min^-1 升温至280℃,保持7 min;进样口温度240℃;采用质谱检测器,电子轰击源EI,离子源温度230℃,采用多反应监测模式。结果: 采用所建立的方法对海藻羊栖菜进行检测,对照品与供试品中相邻色谱峰分离情况均良好,除六氯苯外,其他有机氯农残加样回收率均在72%～127%之间,RSD也满足要求。未检出羊栖菜样品中含有有机氯农药残留。结论: 方法的建立为海藻类样品有机氯农药残留检测提供了参考。     

重组人胰岛素外源性DNA的荧光法测定

目的建立重组人胰岛素外源性DNA残留量的荧光检测方法,用于重组人胰岛素的质量控制。方法参照《中国药典》三部附录及相关资料方法,对样品的处理方法、测定方法等方面研究了外源性DNA残留的荧光法检测。从标准曲线、加样回收率、精密度、耐用性、重复性等方面进行了荧光法的方法学研究。结果建立了重组人胰岛素原料药中外源性DNA残留量的荧光检测方法,并进行了方法学验证。结论该方法具有简便、快速、重复性好等特点,可用于重组人胰岛素的外源性DNA残留量检定。     

关于中药评价性抽验中探索性研究的几点思考

从处方、制备工艺、质量标准、特殊类药材和外源性有害物质的控制、包装材料的相容性、现代分析技术及分析手段和数学方法的应用及针对中药注射剂的研究等几方面对国家中药评价性抽验中的探索性研究工作进行探讨,提出一些想法供同行参考。     

风轮菜属药用植物研究进展

目的对唇形科风轮菜属药用植物的研究进展进行综述,为风轮菜属药用植物的进一步研究提供参考。方法查阅国内外最近十几年的数十篇文献资料,从化学成分类型、分类学研究、药理作用、临床应用等方面对风轮菜属药用植物的研究进展进行综述。结果与结论风轮菜属植物主要含有黄酮、皂苷、有机酸、芳香族化合物、三萜、甾体等多种化学成分,其中黄酮类和皂苷类化合物为该属植物的主要活性成分。对风轮菜属10种植物用高效液相色谱与系统聚类分析方法进行分类,其结果符合植物分类学的结论,Calamintha glandulosa更接近于Micromeria属。风轮菜属药用植物具有止血、抗菌、抗炎及免疫、抗肿瘤、抗辐射等药理活性,临床主要用于治疗功能性子宫出血等。风轮菜属药用植物有进一步开发的药用价值。     

选育羊栖菜与野生羊栖菜中褐藻胶与褐藻糖胶组成分析

目的比较选育羊栖菜(H.fusiformis)与野生羊栖菜中褐藻胶与褐藻糖胶的组成差异。方法采用高效凝胶渗透色谱法(HPGPC)分析多糖相对分子量,用核磁共振氢谱法测定褐藻胶中G/M比,并用高效离子色谱(HPIC)法分析褐藻糖胶中单糖组成。结果选育羊栖菜和野生羊栖菜中褐藻胶和褐藻糖胶含量分别为29.23%,1.89%和32.18%,2.40%;褐藻胶中G/M比分别为2.62和1.05;褐藻糖胶均含有8种单糖,分别为岩藻糖,半乳糖,甘露糖,葡萄糖醛酸,葡萄糖,木糖,葡萄糖胺和甘露糖醛酸,其摩尔比分别为34.62,18.55,14.17,12.72,10.60,5.79,2.42,1.13及34.76,19.26,10.21,12.70,5.49,10.22,0.70,6.66。结论选育羊栖菜褐藻胶中古罗糖醛酸含量以及褐藻糖胶中葡萄糖,甘露糖和氨基葡萄糖含量均明显高于野生羊栖菜。     

中药外源性有害物质分析与研究

中药外源性有害物质已受到广泛关注，严重影响中药质量，危害人类健康。影响中药质量安全的因素主要包括真菌毒素、农药残留、重金属及有害元素三方面。本文针对以上三个方面分别对其毒理研究、现行标准、检验检测手段等进行归纳总结，并提出相关的建议与意见，为中药质量安全控制体系的完善与提升提供有益的参考。     

Safety of botanical ingredients in personal care products/cosmetics

The key issue of the safety assessment of botanical ingredients in personal care products (PCP) is the phytochemical characterisation of the plant source, data on contamination, adulteration and hazardous residues. The comparative approach used in the safety assessment of GM-plants may be applied to novel botanical PCP ingredients. Comparator(s) are the parent plant or varieties of the same species. Chemical grouping includes definition of chemical groups suitable for a read-across approach; it allows the estimation of toxicological endpoints on the basis of data from related substances (congeneric groups) with physical/chemical properties producing similar toxicities. The Threshold of Toxicological Concern (TTC) and Dermal Sensitisation Threshold (DST) are tools for the assessment of trace substances or minor ingredients. The evaluation of skin penetration of substances present in human food is unnecessary, whereas mixtures may be assessed on the basis of physical/chemical properties of individual substances. Adverse dermal effects of botanicals include irritation, sensitisation, phototoxicity and immediate-type allergy. The experience from dietary supplements or herbal medicines showed that being natural is not equivalent to being safe. Pragmatic approaches for quality and safety standards of botanical ingredients are needed; consumer safety should be the first objective of conventional and botanical PCP ingredients.     

Genetic toxicology in industrial practice: general introduction

During the past decade, important position statements on mutagenicity testing have been issued by industrial organizations such as CEFIC (the European Council of Chemical Industry Federations) and ECETOC (the European Chemical Industry Ecology and Toxicology Centre). Mutagenicity testing is of potential value as a research tool for screening new compounds, as a probe for the identification of harmful substances and as a diagnostic tool for monitoring the health of individuals exposed to certain chemicals. The problems inherent in mutagenicity testing include specificity and sensitivity, and meaningful interpretation of test data will depend on the strict maintenance of accepted quality standards.     

国产注射用硫酸头孢匹罗质量评价

的 评价国产注射用硫酸头孢匹罗的质量现状并分析存在的问题。方法 按照2017年国家评价性抽验计划总体要求,采用法定检验方法进行样品检验,并结合探索性研究进行统计分析,对国产注射用硫酸头孢匹罗的质量现状进行评价。结果 本次抽验中涉及4家生产企业的12批样品,按法定标准检验结果均符合规定,合格率100%。标准检验发现4个现行标准均为局颁注册标准,存在限度不统一、安全性项目(如聚合物、碳酸钠含量、硫酸盐含量等)缺失或方法不完善等问题。探索性研究显示,由于处方中含有碳酸钠,导致本品有较强的引湿性,引湿后杂质含量明显增加。结论 目前国产注射用硫酸头孢匹罗总体质量较好,质量标准有待统一提高。建议优化有关物质Ⅰ的检查方法,并增加碳酸钠含量和有关物质Ⅱ等安全性项目。     

《中华人民共和国药典（2015年版）》中中药部分的增、修订情况简介

本文简要介绍《中华人民共和国药典（2015年版）》中中药部分的增、修订情况及技术特点。本版药典不仅中药收载品种数大幅增加,而且进一步加强了多药味（成分）的检测、活性成分的控制和杂质（有害物质）的检查,更注重现代分析技术的应用,包括广泛应用了指纹（特征）图谱技术,对提高中药的安全性及其质量整体控制水平具有重要作用。     

The role of laboratory terrestrial model ecosystems in the testing of potentially harmful substances

A classification of terrestrial model ecosystems (TMEs) was introduced which is based upon the physical properties of intactness of the physical medium and openness to the atmosphere. This gave rise to four types of system, namely open and closed intact systems and open and closed homogeneous' systems. These systems have different capabilities with respect to fate and effect end-points with various substances. The large closed TMEs are generally very complex, require a high degree of operator skill, expensive and therefore not replicable. Whilst these can provide estimates of losses due to volatility, they are not useful for determining effect end-points because of low replicability; high replicability being necessary because of natural variation in organism response. Open systems, especially those having intact soil-cores, are usually smaller, less complex and therefore more replicable. These have provided useful information on integrative functional effect end-points, but can only produce mass balances with non-volatile substances. Homogenization of the medium has also helped elucidate ecotoxicological effects by increasing replicability, but may introduce artifacts because of the disruption to soil organisms.A major limitation of TME studies would seem to be that few effect end-points can be non-destructively sampled. Further investigations into these may provide information on recovery of terrestrial ecosystems over time after substance application, perhaps using multivariate statistical techniques. Other problems concerning TMEs are related to complexity and scale. In this respect ecosystem functions in which microorganisms play a major role, such as nutrient cycling, provide the greatest similarity when compared to field evaluations of the same substances, especially where the TME is intact. However, effects upon structural aspects of biological communities have in general not been well researched in TMEs. Once these have been added to the more complete set of functional end-points, TMEs will provide a very useful tool in hazard assessments of potentially harmful substances.     

The FEMA GRAS assessment of alpha,beta-unsaturated aldehydes and related substances used as flavor ingredients

This publication is the 12th in a series of safety evaluations performed by the Expert Panel of the Flavor and Extract Manufacturers Association (FEMA). In 1993, the Panel initiated a comprehensive program to re-evaluate the safety of more than 1700 GRAS flavoring substances under conditions of intended use. Since then, the number of flavoring substances has grown to more than 2200 chemically-defined substances. Elements that are fundamental to the safety evaluation of flavor ingredients include exposure, structural analogy, metabolism, toxicodynamics and toxicology. Scientific data relevant to the safety evaluation for the use of aliphatic, linear alpha,beta-unsaturated aldehydes and structurally related substances as flavoring ingredients are evaluated. The group of substances was reaffirmed as GRAS (GRASr) based, in part, on their self-limiting properties as flavoring substances in food; their low level of flavor use; the rapid absorption and metabolism of low in vivo concentrations by well-recognized biochemical pathways; adequate metabolic detoxication at much higher levels of exposure in humans and animals; the wide margins of safety between the conservative estimates of intake and the no-observed-adverse effect levels determined from subchronic and chronic studies. While some of the compounds described here have exhibited positive in vitro genotoxicity results, evidence of in vivo genotoxicity and carcinogenicity occurs only under conditions in which animals are repeatedly and directly exposed to high irritating concentrations of the aldehyde. These conditions are not relevant to humans who consume alpha,beta-unsaturated aldehydes as flavor ingredients at low concentrations distributed in a food or beverage matrix.     

X射线荧光光谱法在药品元素杂质分析中的应用

X射线荧光光谱（X-ray Fluorescence Spectrometry,XRF）是基于测量由初级X射线激发的原子内层壳电子产生的特征X射线光量子的一种仪器分析方法。本文介绍了XRF的分类、特点和各国药典标准,综述了国内外XRF在药品研发以及原料药、药用辅料和制剂元素杂质分析中的应用进展,以期为药品的元素杂质控制研究提供参考。     

Role of FOSHU (food for specified health uses) for healthier life

Proper combination of diet, exercise and rest is important for healthier life. Concerning diet in particular, proper balance of nutrient intake and avoidance of its excess or deficiency are essential to keep good health and thus, not to induce risks leading to lifestyle-related diseases. Even nutrients and functional ingredients in foods are chemical substances but we need to draw a line of demarcation between such substances based on long history of dietary habits and novel substances and/or xenobiotics. However, even FOSHU contains highly purified or concentrated functional ingredients present in ordinary foods and thus, it is very important to take safety issues into consideration. FOSHU is the only type of food product (not ingredients) that can carry health claims and is composed of functional ingredients that affect the structure/function (physiological functions) of the body. These food products are intended to be consumed for the maintenance/promotion of health or special health uses by people who wish to control specified health conditions, such as gastrointestinal conditions and blood pressure. Therefore, FOSHU products target healthy people and people in a preliminary stage of a disease or a borderline condition. When the products are manufactured or distributed, permission or approval from the government is required after rigorous evaluation of the safety and effectiveness of proposed specified health uses. To understand the outline overall, comprehensive knowledge on maintaining health is required, i.e., structure/function of human body, pathogenesis of diseases, role of dietary life, nutrients and their metabolism etc., as well as understanding mechanisms of the effectiveness of FOSHU, which ranges over pharmacology, medicine, and food and nutrition.     

抗感染药物杂质对照品的研发策略与展望

摘要：杂质研究是药品质量控制的热点,也是当前药品注册审评审批中所关注的重点。随着药物分析、检测技术的提高, 药品质量标准中对杂质的控制水平也不断提高,进而对杂质分析中特定杂质的定位、定量以及复杂分析方法的转移、评价提出 了新的挑战。采用适宜的杂质对照品可以较好地解决上述难题。本文以杂质或组分相对复杂的抗感染药物为例,重点介绍了中 检院通过研制特定杂质对照品和混合杂质对照品,尝试解决上述问题的思路,提出杂质对照品的研发策略,并阐述目前存在的 问题和今后的发展方向。     

Formulation design for poorly water-soluble drugs based on biopharmaceutics classification system: basic approaches and practical applications

The poor oral bioavailability arising from poor aqueous solubility should make drug research and development more difficult. Various approaches have been developed with a focus on enhancement of the solubility, dissolution rate, and oral bioavailability of poorly water-soluble drugs. To complete development works within a limited amount of time, the establishment of a suitable formulation strategy should be a key consideration for the pharmaceutical development of poorly water-soluble drugs. In this article, viable formulation options are reviewed on the basis of the biopharmaceutics classification system of drug substances. The article describes the basic approaches for poorly water-soluble drugs, such as crystal modification, micronization, amorphization, self-emulsification, cyclodextrin complexation, and pH modification. Literature-based examples of the formulation options for poorly water-soluble compounds and their practical application to marketed products are also provided. Classification of drug candidates based on their biopharmaceutical properties can provide an indication of the difficulty of drug development works. A better understanding of the physicochemical and biopharmaceutical properties of drug substances and the limitations of each delivery option should lead to efficient formulation development for poorly water-soluble drugs.