Blood glucose is a direct indicator for diagnosis and discrimination of diabetes, and reference materials are important guarantee for the accuracy and comparability of blood glucose detection results.The process of developing glucose in human serum reference materials with six different concentration levels includes the preparation, value determining, uniformity, stability test, uncertainty evaluation and interoperability evaluation of reference materials. Two different principles of isotope dilution liquid chromatography tandem mass spectrometry and isotope dilution gas chromatography mass spectrometry were used to determine the concentration value of glucose in human serum, and the differences and causes between the analysis results of the two methods were analyzed. The quantitative value of glucose in human serum reference material at different concentration levels in human serum covers 1.70～28.12 mmol/L. This series of reference material have good uniformity and stability, and have obtained the gradation certificate of national secondary certified reference material, the number is GBW（E） 091140～GBW（E） 091145, which are expected to be used in clinical tests and related areas for quality evaluation of measurement of serum glucose items and other aspects.

本文介绍了6个水平人胰岛素溶液标准物质的制备、定值、均匀性和稳定性检验等研制过程.该系列标准物质以GBW09292胰岛素(人)纯度国家一级标准物质为原料,通过重量-容量法,采用天平准确称重并定容到容量瓶中,配制出6个水平的人胰岛素溶液标准物质候选物;接着在洁净环境下将标准物质候选物分装到棕色安瓿瓶中,每管分装500μL,置于-70℃冰箱中冷冻保存.以重量-容量法的配制值作为定值结果,不确定度评定时考虑了配制过程中由天平、容量瓶引入的不确定度分量,以及由仪器检出限和标准物质均匀性及稳定性引入的不确定度分量.研制的6个水平人胰岛素溶液标准物质均匀性良好,在-70℃可保存6个月,在4℃时可以至少稳定一周.该系列标准物质主要配合JJF1752-2019《全自动封闭型发光免疫分析仪校准规范》,用于仪器重复性、线性、交叉污染率计量特性的评价.该系列标准物质的研制,将有助于相关仪器校准工作的开展.

A mass balance method and a high performance liquid chromatography-isotope dilution mass spectrometry (HPLC-IDMS)method are established to determine the mass fraction of pure human serum albumin(HSA). With the mass balance method,the pure HSA is quantified by HPLC and its moisture and ash are quantified by Karl Fischer and ignition residue analysis,which give an average mass fraction of 0. 861 g/g. By the HPLC-IDMS method,after the pure HSA is hydrolyzed by acid,the resulted Pro,Val and Phe are quantified. Consequently,the mass fraction of HSA is calculated by the average. Under the optimized conditions,the mass fraction of HSA is 0. 853 g/g with a relative standard deviation(RSD)of 0. 8% and an expanded uncertainty of 0. 015 g/g(k = 2). The limits of detection and quantification are 1. 37 í 10 - 5 g/g and 4. 55 í 10 - 5 g/g,respectively. Compared with the mass balance method,the relative bias of the HPLC-IDMS method is 0. 9% .

参加了澳大利亚计量院组织的麸质蛋白过敏原ELISA定量测定能力验证,采用德国拜发公司的醇溶蛋白试剂盒进行测定,所得醇溶蛋白含量标准曲线的相关系数r2=0.9961,线性范围(0 ～ 40) ng/g.通过醇溶蛋白含量的两倍计算麸质蛋白的含量,并对测定结果的不确定度进行了评估.多次测得样品中的麸质蛋白的平均含量为18.9μg/g,日内变异系数为3.13％ ～3.76％,日间变异系数为4.45％,相对扩展不确定度为23.8％.返回结果表明测定数据处于等效区间,证明了实验室已具有较好、国际等效的麸质蛋白过敏原定量测定能力.

<正>一、概述牛血清白蛋白第V组分(BSA)是牛血清中的一种球蛋白,包含583个氨基酸残基,分子量约为66430,等电点为4.7。牛血清白蛋白广泛应用于生化实验中,也是最常用的蛋白质定量的标准。为了保证我国蛋白质含量测定结果的准确、可比与可溯源,中国计量科学研究院率先采用同位素稀释质谱法和纯度扣除法研制了牛血清白蛋白固体国家一级标准物质,定值结果为(0.963±0.038)g/g。但

<正>蛋白质含量通常采用氨基酸分析法、凯氏定氮法、比色法、紫外分光光度法等进行测定。蛋白质含量的荧光分析法是近年来发展起来的蛋白质含量分析方法,具有灵敏度高、线性范围宽等特点。采用荧光法测定蛋白质含量

The importance of setting up traceability from protein content result to SI unit was stressed.Based on the development of international and domestic protein metrology research,two possible ways were proposed for setting up the traceability.In the proposed ways,protein content result can be linked to SI unit by authoritative methods such as isotope dilution method,titration method,freezing point method and so on.That will ensure the accuracy and traceability of protein content result.The value can be delivered to application fields with protein certified reference materials as value carrier.Therefore,the value traceability and delivery system for protein content can be set up.

<正>近年来,随着生命科学及生物产业的迅速发展,生物计量已经作为一个崭新的计量领域被提到日程上来。蛋白质计量作为生物计量的一个重要分支,已经成为生物计量研究的焦点之一。国际物质量咨询委员会(CCQM)生物分析工作组(BAWG)于2001年确定的蛋白质计量研究内容包括蛋白质定量、氨基酸序列及大小(相对分子质量)、蛋白质功能、活性以及蛋白质的高级结构等。

The presented work is to determine the mass fraction of angiotensinⅠ in solution by isotope dilution method,which is a pilot study organized by Consultative Committee for Amount of Substance.Firstly,the hydrolysis time and hydrochloric acid addition volume ratio were optimized and the degradation of natural and isotope labeled proline,valine,leucine and phenylalanine during the hydrolysis process were investigated.Secondly,the mass fractions of proline,valine,isoleucine and phenylalanine in the angiotensinⅠhydrolysis solution was determined employing isotope dilution method with their reference materials as standards.Finally,the angiotensinⅠ mass fraction and associated uncertainty were calculated according to the amino acid mass fraction obtained,which was(75.2±2.6) μg/g.It showed that the result obtained in this paper has good equivalence with the average.It can be concluded that the isotope dilution method for peptide quantification is accurate and is suitable for peptide reference materials production.