101600例0～17岁人群末梢血铜元素参考值的研究

为确定全国0～17岁不同年龄组人群末梢血铜元素含量正常参考值范围,采用火焰原子吸收光谱法检测了来自全国8个省区的101 600名0～17岁健康个体末梢血中铜元素的含量,用百分位数法确定其参考值范围.结果表明,取第5 、第97百分位数值分别作为参考值下限和上限,参考值范围依次为:0岁:8.51～25.63 μmol/L,...     

口腔粘膜免疫性疾病患者血清微量元素变化研究

选择了４５例免疫性口腔粘膜病人进行血清微量元素含量变化研究，以探讨日腔粘膜免疫性疾病患者血清微量元素的变化，给临床提供使用微量元素作辅助治疗的实验依据。结果显示血清锌、铜含量均显著低于对照参考值（Ｐ＜０．０１ｆ）．铁含量低于参考值（０．０１＜Ｐ＜０．０５），而血清镁含量高于对照参考值（Ｐ＜０．００１）。     

乙醛酸缩氨基硫脲和锌（Ⅱ）、铅（Ⅱ）、铜（Ⅱ）、锰（Ⅱ）、镍（Ⅱ）、钴（Ⅱ）配合物的薄层色谱与紫外光谱的研究

用正相薄层色谱法研究了乙醛酸缩氨基硫脲和锌（Ⅱ）、铅（Ⅱ）、铜（Ⅱ）、锰（Ⅱ）、镍（Ⅱ）、钴（Ⅱ）配合物的色谱行为，各组分配合物的比移植Ｒｆ相差较大，得到了满意的分离。讨论了该系列配合物正相吸附薄层色谱比移植与紫外光谱Ｒ带λ（ｍａｘ）变化关系的一致性。     

乙醛酸缩氨基硫脲和锌（Ⅱ）、铅（Ⅱ）、铜（Ⅱ）、锰（Ⅱ）、镍（Ⅱ）、钴（Ⅱ）配合物的薄层色谱与紫外光谱的研究

 用正相薄层色谱法研究了乙醛酸缩氨基硫脲和锌（Ⅱ）、铅（Ⅱ）、铜（Ⅱ）、锰（Ⅱ）、镍（Ⅱ）、钴（Ⅱ）配合物的色谱行为，各组分配合物的比移植Ｒｆ相差较大，得到了满意的分离。讨论了该系列配合物正相吸附薄层色谱比移植与紫外光谱Ｒ带λ（ｍａｘ）变化关系的一致性。     

X—射线荧光光谱分析基本参数法程序在微型计算机上的移植和应用

本文介绍了ＦＬＹ－ＦＰＭ Ｘ－射线荧光分析基本参数法程序在微型计算机上的移植和应用情况。移植程序采用标准ＦＯＲＴＲＡＮ７７程序设计语言编写，适用于ＩＢＭ ＰＣ系列微型计算机。移植程序保留了原程序的所有功能和特点，可以根据需要进行基本参数法、理论α系数法和基本参数法－理论α系数法联用方法的分析计算。对移植程序进行了严格计算验证，程序移植前后计算结果一致，计算速度有所提高。本文给出了高温合金、水泥粉末     

101600例0～17岁人群末梢血锌元素参考值研究

为确定我国0～17岁不同年龄段健康人群末梢血锌参考值范围,采用BH 5100型多通道火焰原子吸收光谱仪检测了全国8省份101 600例0～17岁人群全血锌元素含量,用百分位数法确定末梢血锌元素参考值范围.结果表明,不同年龄段人群末梢血锌元素参考值范围分别是:0岁～,38.38～80.06 μmol/L;1岁～,47.7...     

HBTMPTP与伯胺N1923对稀土元素(Ⅲ)的协同萃取

研究了二（2，4，4-三甲基戊基）单硫代膦酸（HBTMPTP，HL）和伯胺N1923的正己烷溶液从硫酸介质中对稀土元素（Ⅲ）的协同萃取．并以La（Ⅲ）为例，用斜率法、恒摩尔法和饱和法确定了协萃配合物的组成为（RNH3）3L2La（SO4）2，计算了协萃配合物的生成常数及热力学函数，观测了协萃配合物的IR谱．     

悬浮体制样石墨炉原子吸收光谱法直接测定食品中的Cu、Zn、Mn

本文提出以PTFE作为化学改进剂，悬浮体制石墨炉原子吸收光谱法（GFAAS）测定食品中痕量Cu、Zn、Mn的新方法，对GFAAS测定Cu、Zn、Mn的条件进行了优化。在选定的实验条件下，测定Cu、Zn、Mn的特征捏分别为3．1pg,0.8pg和1．8pg。采用水溶液工作曲线法直接分析了食品试样中的痕量Cu、Zn、Mn，其测定结果参考值相一致，本方法无需任何化学前处理，灵敏，简便，快速。     

聚三氟氯乙烯化学改进剂在电热蒸发(ETV)-ICP-AES直接测定生物试样中微量钛的应用

本文首次提出以聚三氟氯乙烯（ＰＴＦＣＥ）为化学改进剂，应用于悬浮体制样ＥＴＶ－ＩＣＰ－ＡＥＳ直接测定固体生物试样中微量钛。实验采用５％ＰＴＦＣＥ，促进Ｔｉ的蒸发。方法的绝对检出限为２ｐｇ（按５σ计），ＲＳＤ为２．６％（ｎ＝５）。该法用于直接测定ＧＢＷ０８５０５茶叶粉末样品中的Ｔｉ，结果与参考值吻合，回收率为９７．３～１０５．４％。     

编者的话--切盼我国的人体头发和血液微量元素正常参考值诊断标准早日出台

本期发表了我国资深的微量元素与健康研究科学家、中国微量元素科学研究会名誉理事长秦俊法教授等撰写的“人体头发和血液微量元素正常参考值的确定原则及方法”论文，这篇文章在目前形势下发表有非常积极的意义。我国搞微量元素与健康研究、微量元素与临床应用研究30多年，发表了有关人体头发和血液微量元素正常参考值论文几千篇，出版了人体微量元素数据手册近十种版本，建立了两个国家级的微量元素数据库，积累了数以百万计人体及其他生物的微量元素数据。各省市也陆续出台了地方性的人发和血液微量元素正常参考值，这些参考值已应用了30多年，接受了临床实践检验30多年。     

Determination of Assigned Values for Cadmium,Cobalt and Manganese in Drinking Water Proficiency Testing

In proficiency tests the selection of an appropriate assigned value is one of the most critical points. Determination of the assigned value for proficiency test can be done in 2 ways: based on reference value and consensus value. The use of such a consensus value as an assigned value is a commonplace in proficiency testing, because there is seldom at present a cost effective alternative. However, the consensus value has a weakness in that it could be significantly different from the true value due largely inexperienced laboratories. Therefore in this work, the reference values were used as the assigned values for all analytes of interest. The reference values in spiked drinking water samples were produced by the Metrology in Chemistry Laboratory of Research Center for Chemistry - Indonesian Institute of Sciences (RCChem-LIPI) with traceable to SI units through standard solutions from the National Institute Standard and Technology, USA. The reference values of cobalt and manganese were obtained by measurement using two from three comparable methods of Graphite Furnace-Atomic Absorption Spectrometry (GF-AAS), Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) while that for cadmium was obtained by a primary method of ICP-Isotope Dilution Mass Spectrometry (ICP-IDMS).The obtained reference values were used to evaluate the laboratory performance result in a proficiency testing scheme of cadmium, cobalt and manganese in drinking water which was provided in 2014. All fifty nine laboratories reported cadmium and cobalt at low concentration levels which were about more than 82% showed satisfactory performance results. Similarly, the results of manganese were also comparable at high level concentrations.     

甲基对硫磷溶液标准物质的研制

采用重量–容量法研制了1.00 ng/μL甲基对硫磷农药标准物质,对研制的甲醇中甲基对硫磷溶液标准物质量值进行了均匀性和稳定性检验,对定值结果的不确定度进行了评定。结果表明,该标准物质均匀性良好,在一年内量值没有显著性变化,具有良好的稳定性,定值结果的相对扩展不确定度为3%(k=2)。该标准物质可用于农药残留测量结果的准确性评价。     

Validation study of immunoaffinity column chromatography coupled with solution fluorometry or HPLC for the detection of aflatoxin in peanuts and corn

Neogen Corp. has developed the Neocolumn for Aflatoxin DR for the detection of total aflatoxin by HPLC or solution fluorometry. The purpose of this study was to validate the method under the requirements of the AOAC Research Institute Performance Tested Methods (PTM) program. There are several AOAC Official Methods for detection of total aflatoxin in corn; they consist of rapid and analytical-based methods and two rapid methods (PTMs 030701 and 050901) that have been performance tested by the AOAC Research Institute. A widely used reference method, however, is AOAC Official Method 991.31, which uses immumoaffinity cleanup followed by HPLC or solution fluorometry and is referred to as the reference method in this document. In internal studies, the Neocolumn method coupled with solution fluorometry demonstrated a relative recovery from peanuts of 101.6% of the reference value, with a CV of 3.9% across all levels analyzed; when coupled with HPLC, the Neocolumn method demonstrated a relative recovery from peanuts of 103.0% of the reference value with a CV of 3.5% across all levels analyzed. The Neocolumn method coupled with solution fluorometry demonstrated a relative recovery from corn of 116.9% of the reference value with a CV of 6.1% across all levels analyzed; when coupled with HPLC, the Neocolumn method demonstrated a relative recovery from corn of 91.2% of the reference value, with a CV of 5.4% across all levels analyzed. Calculations were made by comparison with the mean result obtained by the HPLC reference method, which showed respective CV values of 3.9 and 2.0% for recoveries from peanuts and corn, respectively.     

低浓度氮中二氧化硫气体标准物质的制备

以二氧化硫纯度标准物质和高纯氮气为原料,采用与一级标准物质比较法制备了摩尔分数为10~100μmol/mol的氮中二氧化硫标准物质。用二氧化硫分析仪对配制的标准物质进行了机械混匀试验、压力均匀性和时间稳定性试验。结果表明,滚动30~80 min后该标准物质机械混匀良好;经F检验,在10~0.5 MPa范围内该标准物质量随压力变化无显著差异,具有较好的压力均匀性;在–20℃和40℃条件下保存7 d,其量值无显著变化,可满足运输环节量值稳定性要求;在常温下贮存11个月,量值无显著性变化,满足国家二级标准物质稳定性要求。采用与一级标准物质比较法定值,并对定值结果的不确定度进行了评定。研制的低浓度氮中二氧化硫气体标准物质的标准值分别为9.89,55.4,101.2μmol/mol(U_(rel)=2%,k=2),该标准物质满足国家二级标准物质的相关技术要求,可用于仪器校准、测量过程质量控制及分析方法的确认和评价。     

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。     

Purity verification and measurement uncertainty

In chemical analysis, laboratories are required to verify the purity of reference material being used. Also, the contributions from the verification procedure, where significant, have to be included in the estimation of the total measurement uncertainties of the test results. One common verification procedure is to use another source of the same material if an appropriate certified reference material were not available. This involves a comparison test where the purity value of the reference standard is determined using a second source reference standard as the “calibrant”. In normal practice, the standard uncertainty of the purity value of a reference standard is estimated according to the probability distribution function (PDF) of the possible purity values of the reference standard concerned. With the use of Monte Carlo simulation technique, this paper attempted to study the effect of verification process on that PDF and thus the associated standard uncertainty as well. Also, the effects of parameters like the purity of the second source reference standard, the method precision and the acceptable range set for the comparison test on the verification outcome were discussed.     

镉溶液标准物质的研制

介绍镉溶液标准物质的研制过程。以高纯镉为原料,1%硝酸溶液为基体,利用重量–容量和一步稀释法制备镉溶液标准物质。分别采用F检验和回归曲线法对研制的标准物质进行均匀性和稳定性考察。采用电感耦合等离子体发射光谱法与国家一级标准物质比对定值,并对镉溶液浓度量值进行不确定度评定。利用原子吸收分光光度法和电感耦合等离子体发射光谱法对研制的标准物质与国家二级标准物质进行比对。结果表明,研制的镉溶液标准物质的定值结果为100μg/m L,相对扩展不确定度U_(rel)=1.0%(k=2)。该标准物质量值准确且具有溯源性。     

血清中皮质醇成分分析标准物质的研制

皮质醇是一种重要的肾上腺皮质激素,同时也是一种重要的临床诊断标志物,为保证检测结果具有溯源性、可比性和准确性,研制了血清中皮质醇成分分析标准物质。对血清样品进行分离、过滤、混匀、分装,进行均匀性检验、稳定性考察和定值分析。采用超高效液相色谱–同位素稀释串联质谱(UPLC–ID–MS/MS)法进行定值,混合健康男性血清和健康女性血清中皮质醇的定值结果分别为107.63 ng/g(U=1.44 ng/g,k=2),92.24 ng/g(U=1.68 ng/g,k=2)。采用CCQM–K63a比对样品对定值方法进行验证,测量结果在该比对参考值的不确定度范围内。研制的皮质醇成分分析标准物质符合国家一级标准物质技术要求。     

On the use of consensus means as assigned values

An assigned value can be derived by using either a consensus mean or a reference value. It is up to the proficiency testing provider to decide whether the consensus mean or the reference value might be used. If the consensus mean is used, it must be ensured that there really exists a consensus. This requirement is fulfilled if the participants?? results are not biased on average, and there is an agreement between the results with a precision which is fit for the intended use. The best way to avoid potentially ??biased?? assigned values is to use reference values thus ensuring that the assigned value is close to the ??true?? value.     

异辛烷中正十六烷溶液标准物质制备

以正十六烷和异辛烷为原料,采用重量–容量法制备异辛烷中正十六烷溶液标准物质。经过均匀性检验、稳定性考察和量值比较,结果表明该标准物质符合国家二级标准物质的研制要求,标准值为500 ng/μL(Urel=2%,k=2),可作为量值传递的标准,用于气相色谱仪的校准和检定、分析方法评价,以及正十六烷的质量控制等方面。该标准物质已取得国家二级标准物质证书,证书编号为GBW(E)130660。