气相色谱仪验证要点

介绍分析仪器验证的基本概念和主要内容。总结了气相色谱仪验证中设计确认、安装确认、运行确认和性能确认的验证过程和要点,详细介绍了验证内容、具体项目、参考指标、参与人员、时间频次和要点等内容,指出了气相色谱仪验证需要注意的问题,提出了气相色谱仪验证工作的改进建议,为气相色谱仪器验证提供技术参考。     

尿沉渣白细胞标准物质研制

以白细胞(WBC)作为原料,经过固定、分散,制备尿沉渣WBC标准物质。分别采用F检验和回归曲线法评估标准物质的均匀性和稳定性,使用显微镜计数法进行定值,并对标准物质进行不确定度评定。研制的标准物质均匀性和稳定性良好,于2～8℃避光可保存180天。白细胞标准物质水平1,2,3特性值分别为(1 061.1±86.97),(548.8±55.96),(220.5±26.83) cells/μL(k=2)。该系列制备物可作为临床尿液有形成分白细胞分析仪器校准,测量过程质量控制及分析方法的确认和评价检定用标准物质。     

关于增设“分析测试技术与标准化”栏目公告

随着我国标准化领域的不断拓宽,分析测试行业的标准化工作在国家标准化管理委员会的高度重视下,制定了许多标准,并在标准研究方面取得了许多重要的进展,为了及时反映分析测试行业标准化工作取得的成果,促进该行业间的交流与合作,推动我国测试行业标准化工作的发展,本刊拟开设"分析测试与标准化"专栏,以介绍国内外标准化技术在分析仪器、分析测试用试剂与标准物质、分     

乙酰甲胺磷丙酮溶液标准物质的制备及定值

采用乙酰甲胺磷纯度标准物质为原料,以丙酮为溶剂,制备了浓度为1．00mg／mL的乙酰甲胺磷丙酮溶液标准物质,用液相色谱法和气相色谱法进行了确认,A类标准不确定度为0．009％,B类标准不确定度包括标准物质制备、原料纯度、不均匀性和不稳定性引入的不确定度,其量值分别为0．43％,0．10％,0．87％和0．24％,合成不确定度为0．03mg／mL（k=-2）,乙酰甲胺磷丙酮溶液标准物质的浓度为（1．00±0．03）mg／mL。     

血清雌二醇标准物质的研制

介绍高浓度血清雌二醇标准物质的研制。采集的全血不加任何添加剂和抗凝剂,离心分离出血清,分装。采用同位素稀释–液相色谱串联质谱法(ID–LC–MS/MS)对高浓度血清雌二醇标准物质进行定值及均匀性和稳定性检验,对定值不确定度进行了评定。结果表明,高浓度血清雌二醇标准物质定值结果为3.06 ng/g,扩展不确定度为0.08 ng/g(k=2),均匀性和稳定性符合国家标准物质技术要求。采用IFCC RELA比对样品和欧洲标准局标准物质血清17β-雌二醇标准物质对定值方法进行确认,测量结果的标准偏差在该标准物质量值的不确定度范围内。研制的标准物质量值经过日本计量院验证,测量结果为(3.03±0.1)ng/g。该标准物质的量值具有溯源性和准确性。     

没食子酸丙酯纯度标准物质的研究

研制了没食子酸丙酯纯度标准物质。依据国家《一级标准物质研制技术规范》,采用高效液相色谱(HPLC)法和差示扫描量热(DSC)法对没食子酸丙酯纯度标准物质进行联合定值,进行了相应的不确定度评定。研制的没食子酸丙酯纯度标准物质定值结果为(99.8±0.5)%(k=2,P=0.95)。该标准物质可用于相关药品生产及使用单位的质量控制和分析方法确认评价。     

氧、氮、氢分析仪校准方法探讨

建立了氧、氮、氢分析仪的校准方法,介绍了氧、氮、氢分析仪的工作原理、校准要求、校准用标准物质.以北京纳克分析仪器有限公司生产的ON-3000氧氮分析仪和H-3000氢分析仪作为校准对象,对校准方法进行了验证.该方法已作为评价氧、氮、氢分析仪的依据并得到认可.     

我国分析仪器性能测试标准体系框架研究

该文对我国分析仪器性能测试标准化现状和存在的不足进行了分析,根据当前分析仪器性能测试的工作需求提出了符合我国国情的标准体系框架,并在此基础上给出了对我国分析仪器性能测试标准体系建设的建议.     

江苏省色谱专业委员会正式成立

江苏省分析测试协会色谱专业委员会于 2 0 0 2年 5月 17日在南京市江苏省生产力促进中心正式成立。来自全省科研院所、高等院校、中小企业等从事食品、医药、环境、农药等行业的色谱技术人员约 10 0人参加了成立大会。大会由江苏省分析测试协会秘书长夏春阳主持 ,常务理事长姚义刚到会祝贺并发表了讲话。会议选举袁倚盛教授为主任委员 ,戴军、赵厚民、江夕夫和练鸿振为副主任委员。该色谱专业委员会成立后将为江苏省广大色谱类仪器分析测试技术人员组织及举办有关色谱 /质谱仪器的分析测试学术报告会、分析测试技术交流会和分析仪器展示会 ;…     

水中苯甲酸钠标准物质的研制

介绍水中苯甲酸钠标准物质的制备方法。以苯甲酸钠为原料,采用重量–容量法制备溶液标准物质,以液相色谱–紫外可见分光光谱法对标准物质进行均匀性和稳定性检验,并对该标准物质定值结果的不确定度进行评定。结果表明,研制的水中苯甲酸钠标准物质的定值结果为(23.6±0.3) mg/L,有效期为6个月。该标准物质具备良好的均匀性和稳定性,可用于食品防腐剂苯甲酸分析方法的确认与评价。     

A mussel tissue certified reference material for multiple phycotoxins. Part 1: design and preparation

The development of multi-analyte methods for lipophilic shellfish toxins based on liquid chromatography–mass spectrometry permits rapid screening and analysis of samples for a wide variety of toxins in a single run. Validated methods and appropriate certified reference materials (CRMs) are required to ensure accuracy of results. CRMs are essential for accurate instrument calibration, for assessing the complete analytical method from sample extraction to data analysis and for verifying trueness. However, CRMs have hitherto only been available for single toxin groups. Production of a CRM containing six major toxin groups was achieved through an international collaboration. Preparation of this material, CRM-FDMT1, drew on information from earlier studies as well as improved methods for isolation of toxins, handling bulk tissues and production of reference materials. Previous investigations of stabilisation techniques indicated freeze-drying to be a suitable procedure for preparation of shellfish toxin reference materials and applicable to a wide range of toxins. CRM-FDMT1 was initially prepared as a bulk wet tissue homogenate containing domoic acid, okadaic acid, dinophysistoxins, azaspiracids, pectenotoxin-2, yessotoxin and 13-desmethylspirolide C. The homogenate was then freeze-dried, milled and bottled in aliquots suitable for distribution and analysis. The moisture content and particle size distribution were measured, and determined to be appropriate. A preliminary toxin analysis of the final material showed a comprehensive toxin profile.     

Need and use of reference materials in a comprehensive countrywide monitoring of radionuclides

The reliability of measurement results is essential for forming a common database of a laboratory network, because a well-maintained and consistent database is the crucial point of countrywide monitoring. Reference materials are important tools in realizing some aspects of quality assurance; they are especially useful in harmonizing work within the network. Among usual types of reference materials in radio analytics solutions, matrix reference materials and some special reference objects are used. All classes of reference materials should be used depending on the purpose of the demonstration of quality, even in-house reference materials. Interlaboratory measurement comparison and performance evaluation programs play important quality assurance role in radio analytical laboratories. Fortunately, nowadays, the main task is to determine a very low radioactivity concentration in the environment; therefore, pre-concentration is necessary. Generally, the radionuclide bearing natural materials collected from sites where there had been sufficient time for natural processes to redistribute various chemically different species of radionuclides are more reliable reference materials than spiked materials—the main difference is the chemical bounding which is crucial from the point of view of the bioavailability. The need of reference material is summarized according to the intended use, like quality control, measurement validation, and instrument calibration.     

Production and stability testing of incurred reference materials for the anabolic steroid trenbolone in bovine urine.

The production of stable reference materials with incurred residues of veterinary drugs is necessary for the validation of methods of analysis, including the determination of critical performance characteristics. A reference material for trenbolone in bovine urine was produced and the long-term stability was tested. From a pilot 16 week stability study on seven batches containing different additives it was concluded that the use of preservatives does not improve the stability of the residue. A final batch of reference material of 800 vials each containing 5 ml of urine with a target concentration of 5 micrograms l-1 was prepared. The homogeneity and long-term stability of the material were tested. The material was found to be homogeneous. Based on the results of a 52 week stability study it was concluded that the material is stable, using the current analytical methodology. For the development of reference materials, highly accurate and precise analytical methods are necessary. However, the current analytical methodology is not suitable for full evaluation and certification. Currently, a new LC-MS method is being developed. After validation of this method, the stability and homogeneity study will be repeated.     

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。     

Validation of a computer program for atomic absorption analysis

 The approach to validation of a computer program for an analytical instrument as a component of the analytical method (using this instrument with the program) is discussed. This approach was used for validating a new program for atomic absorption analysis. The validation plan derived from this approach was based on minimising the influence of all steps of the analytical procedure on the analytical results obtained by the method. In this way significant changes in the results may be caused only by replacement of the previous program by the new one. The positive validation conclusion was based on the comparison of the results of the analysis of suitable reference materials obtained with the new program and with its precursor in the same conditions, and also on comparison of their deviations from the accepted reference values for these materials, with the corresponding uncertainties. Received: 25 January 1997 Accepted: 14 March 1997     

Referencing strategies and techniques in stable isotope ratio analysis

Stable isotope ratios are reported in the literature in terms of a deviation from an international standard (delta-values). The referencing procedures, however, differ from instrument to instrument and are not consistent between measurement facilities. This paper reviews an attempt to unify the strategy for referencing isotopic measurements. In particular, emphasis is given to the importance of identical treatment of sample and reference material ('IT principle'), which should guide all isotope ratio determinations and evaluations. The implementation of the principle in our laboratory, the monitoring of our measurement quality, the status of the international scales and reference materials and necessary correction procedures are discussed.     

Determination of trace levels of iron in a seawater sample using isotope dilution/inductively coupled plasma mass spectrometry.

An analytical method for trace levels of iron in a seawater sample using isotope dilution ICP-MS was developed. Preconcentration of iron and the removal of major elements in seawater such as alkali and alkaline-earth elements can be carried out quickly using a chelating resin disk by adjusting the sample pH to 3. The collision cell option of the ICP-MS instrument method was used to improve the performance of the instrument for iron measurements since ArO and ArN interferences could be reduced using this analytical method. About 4 ml min(-1) helium, as the collision gas, were introduced into the cell. 40Ar14N and 40Ar16O which interfere with 54Fe and 56Fe in water had their amounts decreased by 5 orders of magnitude. Then, the isotope dilution method was used for iron determination below ng g(-1) level of trace iron in four environmental reference materials (river water standard sample JAC-0031 (Japan Soc. for Analytical Chemistry), estuarine standard sample SLEW-2 (NRC Canada) and seawater standard samples CASS-3 and NASS-5 (NRC Canada)) were measured. Good agreement between analytical results and certified values of reference materials was obtained, which confirmed the effectiveness of this method.     

Analytical instrument qualification in capillary electrophoresis

Capillary electrophoresis (CE) is a well-established and frequently used technique in the pharmaceutical industry. Therefore an appropriate analytical instrument qualification (AIQ) is required for quality assurance. AIQ forms the basis of a quality management followed by analytical method validation, system suitability tests (SSTs) and quality control checks. Two parts of the AIQ, namely the operational qualification (OQ) and the performance qualification (PQ) are of particular interest in the daily routine of the laboratory. A new concept for OQ and PQ was developed to assure the correct function of a CE system. The significance of each parameter, possible test methods as well as acceptance criteria will be presented and discussed in detail. Especially temperature adjustment by the cooling system and the voltage supply must be tested for accurate and precise operation. The detector noise, wavelength accuracy and detector linearity have to be checked as well. Finally, the injection linearity, accuracy and precision need to be qualified. The proposed set of qualification procedures is easy to implement and was already tested on five CE instruments from three different manufacturers. A time- and cost-saving continuous PQ was derived, using results from method-specific SSTs and some additional experiments. This holistic concept continuously surveys the most relevant parameters, hence assuring the suitability of the used instruments and decreasing their downtimes.     

Moderated pressure microwave digestion system for preparation of biological samples

A new type closed digestion vessel was constructed for digestion of biological samples. In this the vapour pressure can be maintained on moderated level (150-300 kPa) by means of an internal cooling spiral. During the operation the reflux of the condensed acid and water vapour continuously renews the liquid phase over the sample. By this way a less expensive microwave system may be applied. The performance of this instrument is practically equal to the commercial systems. The digestion time of plant and tissue samples is 5-10 min and the analytical results for reference materials are in good agreement with the reference values.