化学分析方法验证和确认的应用研究

分析方法的验证/确认是实验室引进新方法时必做的工作,也是实验室技术工作的重点和难点之一。对实验室采用分析方法的验证和确认工作进行归纳总结,详述了分析方法选择性、测量范围、线性范围、检出限和定量限、精密度、准确度的验证/确认方法及结果判定方式。适用于实验室引进的标准方法(包括标准变更)和非标准方法(实验室设计/制定的方法、超出预定范围使用的标准方法、扩充和修改过的标准方法)的验证和确认。     

色谱类分析仪器性能确认用标准物质的筛选

分析仪器验证是制药、食品、环境等多个行业实验室质量管理的重点,为解决我国色谱类分析仪器验证评价体系中缺乏统一标准物质的问题,提出了筛选性能确认行业推荐用标准物质的原则。通过分析不同行业色谱类分析仪器标准物质使用情况和国家标准及有证标准物质的发布现状,以筛选原则为指导,筛选出93种高效液相色谱性能确认用标准物质。为保证分析仪器的稳定性和可靠性提供了标准依据。     

测量方法确认技术及其指标评价

阐述了测量方法确认的方法、指标以及方法确认的6种技术手段；介绍了方法确认技术的9种指标以及指标的获得和评价；指出方法确认技术的重点应放在识别和消除显著影响方面。     

《色谱技术丛书——色谱定性与定量（第二版）》

要点：本书第二版增强了色谱峰纯度检验,色谱指纹图潜、实验室能力验证和实验室认证与认可等相关内容的介绍。     

气相色谱仪性能验证方法的建立及应用

建立气相色谱仪性能验证新方法,为申请WHO药品预认证提供保障。根据欧洲药品质量管理局《质量控制文件》提供的方法,结合《中国药典》要求,与我国计量检定规程进行对比,总结气相色谱仪性能验证参数要求,建立气相色谱仪性能验证检测方法,并用该方法对5台气相色谱仪进行检测,结果符合实际。     

便携式气相色谱仪的介绍及其在环境污染事故应急监测中的应用

对便携式气相色谱仪及其在环境污染事故应急监测中的应用进展作了评述,涉及的内容有便携式气相色谱仪的进样方式、色谱柱和检测器等性能特点及4种常见型号的便携式气相色谱仪的简介,及其在实际应用中的效果(引用文献21篇)。     

天然气气相色谱仪检定装置的建立

为了保证天然气工业用气相色谱仪分析结果准确可靠和量值溯源有效,依据JJG 1055—2009《在线气相色谱仪》、JJF1033—2016《计量标准考核规范》等规程规范要求,配置建标所需计量标准器,研究开展了重复性试验、不确定度评定、检定结果的验证等工作,建立了天然气气相色谱仪检定装置,通过了国家市场监督管理总局的现场考...     

标准方法的证实和非标准方法的确认

介绍检测和校准方法证实与确认的概念。从版本的有效性、人员、设备、材辅料、样品、作业指导书、设施和环境条件等方面介绍标准方法的证实内容;介绍非标准方法的确认方法、步骤以及非标准方法确认应有的文件和确认记录。列举了非标准方法特性量的测定示例。校准方法的证实与确认能有效确保检测和校准的准确性。     

裂解气相色谱—裂解毛细柱气相色谱联用仪

设计了一种裂解气相色谱--裂解毛细柱气相色谱联用仪。在第一级裂解气相色谱仪把聚合物裂解并分离裂解产物,分离了的产物用六通气体进样阀选取并逐个在第二级裂解气相色谱仪裂解,得到聚合物裂解产物的裂解气相色谱图。与低分子化合物的标准指纹图比较,这些裂解产物就得到确认,这样,就可以充分肯定地推断复杂聚合物的组成。     

气相色谱仪检定装置的使用方法

依据JJG 700–1999《气相色谱仪检定规程》介绍气相色谱仪检定装置的使用方法。检定项目包括载气流速稳定性、柱箱温度稳定性和程序升温重复性、衰减器换挡误差以及检测器的灵敏度。给出了热导检测器(TCD)、火焰离子化检测器(FID)、火焰光度检测器(FPD)、电子俘获检测器(ECD)和氮磷检测器(NPD)检定时的色谱条件及使用注意事项。正确使用气相色谱仪检定装置能保证仪器测量数据的准确可靠。     

Equipment qualification and its application to conductivity measuring systems

It is only possible to obtain analytical results that are suitable for their intended purpose if the equipment used is capable of producing measurements of the required quality. To ensure that this requirement is met, analysts should define the performance criteria required from the instruments, ensure that only suitable instruments are selected for analytical measurements, and confirm that these instruments continue to meet these criteria for their entire operational life. This process should be conducted on a formal, documented basis, known as equipment qualification. In addition to describing the key elements of equipment qualification for all analytical instruments, this paper gives specific guidance on its application to conductivity systems that has never previously appeared in the literature. The benefits of performing equipment qualification are highlighted and guidance is given on the selection of control standards and why the equipment vendor performing stages of equipment qualification can be of benefit to the user. The relationship between equipment qualification and method validation is discussed, including how these activities play a major role in determining the quality control measures that should be applied to routine analysis.     

Selecting parameters and limits for equipment operational qualification

While operational qualification (OQ) is a well-established term within equipment qualification, users of equipment often become unsure when it comes to implementation. The biggest problem is how to select procedures and acceptance criteria. Should these be the vendor's specifications or should the users define their own limits, and, if so, how? Should all instruments of the same type have the same values or should these be optimized for each individual instrument? This article will provide an overall strategy and specific examples for HPLC on how to select procedures and acceptance limits that are based on efficient use of resources, on practicality and on the intended use of the equipment.     

The development and application of guidance on equipment qualification of analytical instruments

 This paper describes the development of guidance for the equipment qualification (EQ) of analytical instruments. EQ is a formal process that provides documented evidence that an instrument is fit for its intended purpose and kept in a state of maintenance and calibration consistent with its use.     

微型集成化色谱仪

用微制造技术和色谱原理结合，以全新的概念和设计思维研制色谱仪一微型集成化色谱仪。这种仪器的整个色谱部分在基片上制成。集微型进样器，细内径毛细管柱和微型固体检测器于一体，功耗不过几瓦，重不过几百克，而分析速度比现有仪器提高近一个数量级，检测灵敏度可达１０＾－６Ｖ／Ｖ。这种仪器的制作过程类似半导体器件，能大批量，性能高度重复可靠、而成本极为低廉地制造出来，彻底改变传统色谱仪器的生产方式。本文给出这种仪     

国内标准物质概况及重点领域发展现状

介绍标准物质的层级分类及重点领域内标准物质的研发现状。标准物质有两种分类方法:术语层级分类和计量学层级分类,国内标准物质按照等级划分为一级、二级标准物质、标准样品和行业标准样品。介绍了标准物质生产资质和标准物质证书的要求,以及重点领域医药、金属、油品、食品、环境标准物质的发展现状。     

气相色谱-质谱法分析橡苔浸膏中的挥发性化学成分

 用挥发油提取器提取橡苔浸膏中的挥发油,利用气相色谱-质谱法(GC-MS)分析了其中的化学成分,采用GC峰面积归一化法定量,鉴定出24种化合物,共占挥发油总量的83%以上     

检测实验室如何开展管理评审工作

详细论述了管理评审的基本概念、如何开展管理评审工作以及中国实验室国家认可委员会的有关政策。     

实验室信息管理系统中仪器设备管理模块的设计与实现

根据资质认定、实验室认可要求, 从仪器设备管理的要求和仪器设备管理工作实际出发, 归纳了实验室仪器设备管理、计量溯源方面的要求以及管理环节中容易出现的问题, 采用用户界面(user interface, UI)插件技术和Gojs技术开发了信息管理系统仪器设备管理模块, 降低了系统维护的难度, 满足了系统使用的个性化需求, 实现了仪器设备的分权限协作管理, 充分满足了资质认定、实验室认可中仪器设备管理的要求, 给仪器设备的使用、维修、维护工作带来了诸多便利, 提高了工作效率, 成为了仪器设备管理的有效工具.     

Trace analysis of alkaline flavors in cut tobacco by heart‐cutting multidimensional GC–GC–MS

Tobacco is a complex chemical matrix. The analysis of trace alkaline flavors in tobacco is very difficult because of the limited peak capacity of monodimensional GC. In the present study, a home‐assembled twin‐oven GC–GC–MS system, with MS detection in both dimensions, has been applied to the analysis of 20 alkaline volatiles in a variety of cut‐tobacco samples. By transferring nine and six heart‐cuts from the first apolar column to the second polar column in two separate runs, the potential mutual interference of adjacent isomeric targets and the complex matrix could be removed. For comparative purposes, a systematic comparison of both quantification and qualification results for the cut‐tobacco sample as quality control was conducted between GC–GC–MS and GC–MS. The results showed that GC–GC–MS provided higher accuracy in peak assignment and quantification. And in GC–MS, the interferences of co‐elution had caused both low matched similarity in peak assignment and false‐negative/‐positive results in quantification for some targets. Advantages of the developed GC–GC–MS method in the analysis of alkaline flavors are its high resolving power, reliability, and simplicity.