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GBW10010a大米标准物质复(研)制及数据特征

Preparation of Reference Materials GBW10010a for Rice Component and Data Characteristics

  • 摘要: 随着我国对生态文明建设的重视,自然资源综合调查势在必行,对生物标准物质亦提出了新的需求。当前相关调研工作已经大面积开展,自然资源综合调查、农产品与食品安全评价都需要对生物样品元素组成进行准确测试,需要以生物标准物质作为生物成分测试量值比对和溯源的基础,因此对生物基体标准物质的需求量大幅增加。大米作为主要粮食之一,其食品安全日益受到重视,对大米中的化学成分进行准确的分析测试具有重要的现实意义,因而对大米标准物质的需求量尤为突出,但目前大米成分分析标准物质已供不应求。本文严格按照《标准物质定值的通用原则及统计学原理》(JJF 1343—2012)和《地质分析标准物质的研制》(JJF 1646—2017)等相关规范要求,开展了GBW10010a大米成分分析标准物质的复(研)制工作,包括样品采集、加工制备、均匀性检验、稳定性检验、多家实验室协作定值测试及不确定度评定等关键环节。结果表明:本次复(研)制的大米标准物质定值成分多样、量值准确可靠,符合国家一级标准物质的要求。GBW10010a共定值54项主微量元素,包括Ag、Al、As、B、Ba、Be、Bi、Ca、Cd、Ce、Co、Cr、Cs、Cu、Dy、Er、Eu、Fe、Gd、Ge、Hg、Ho、K、La、Li、Ho、Mg、Mn、Mo、N、Na、Nb、Nd、Ni、P、Pb、Pr、Rb、S、Sb、Sc、Se、Si、Sm、Sr、Tb、Th、Tl、Tm、U、V、Y、Yb、Zn,其中的39项元素给出了标准值及不确定度,包括Ag、Al、As、B、Ba、Ca、Cd、Ce、Co、Cs、Cu、Dy、Er、Fe、Hg、K、Li、Mg、Mn、Mo、N、Na、Nd、Ni、P、Pb、Pr、Rb、S、Sb、Se、Si、Sm、Sr、Tb、Tl、Y、Yb、Zn;15项元素提供参考值,包括Be、Bi、Cr、Eu、Gd、Ge、Ho、Ho、La、Nb、Sc、Th、Tm、U、V。与原有GBW10010大米标准物质相比较,GBW10010a中As、Cd、Co、Cr、Cu、Hg、Mn、Mo、Ni、Zn等重金属元素含量显著下降,其中Cd、Cu、Zn降幅较大,分别下降约39%、43%、38.7%,一定程度上反映了农田生态环境的改善。本批标准物质定值元素总数量增加了6项,新增定值元素Ag、Nb(Nb给出参考值),并且各项元素不确定度范围整体上有所缩小,如Al、Cd、Cu、Fe、K、Mg、Mo、Na、P、Pb、Se、Zn等对生物易有影响的重要元素,表明了地质分析测试方法技术的进步及定值水平的提高。本批标准物质定值元素涵盖了具有生物效应的大部分主微量元素,适用于农业生态环境地球化学调查与评价、生物样品测试、农产品质量与食品安全评价样品测试时的分析仪器校正、分析方法评价和分析质量监控等多个领域。

     

    Abstract:
    BACKGROUNDWith the increased attention paid for the construction of ecological civilization, a comprehensive survey of natural resources is imperative, and new requirements for biological reference materials have also been put forward. At present, relevant research work has been widely carried out. The comprehensive investigation of natural resources, agricultural products and food safety evaluation all need to accurately test the element composition of biological samples, and biological reference materials are needed as the basis for the comparison and traceability of biological components. The demand for biological matrix reference materials has increased significantly. As one of the main foods, the food safety of rice has been paid more and more attention. It is of great practical significance to carry out accurate analysis of the chemical components in rice. Therefore, the demand for rice is particularly prominent, but the rice reference materials for composition analysis are still lacking.
    OBJECTIVESTo develop rice certified reference material (GBW10010a) and compare it with the data characteristics of GBW10010.
    METHODSThe rice certified reference material (GBW10010a) was prepared in strict accordance with relevant specifications. The collected candidates were prepared through coarse crushing, drying, fine crushing, sieving, blending and other steps. The particle size distribution was detected by BT-9000ST laser particle size analyzer. 15 bottle samples were randomly selected and homogeneity testing was carried out by ICP-MS and ICP-OES, etc. The data were statistically calculated by one-way ANOVA, indicating good homogeneity of the samples. The long-term stability of the standard material under the specified storage conditions was investigated. The linear model was used to evaluate the stability of the sample. The determination of 60 components was carried out by means of ICP-MS, ICP-OES, AFS, COL, VOL, XRF, IC and other Analytical test methods.
    RESULTSThe rice reference material prepared in this research has diverse fixed value components, accurate and reliable measurement values, and meet the requirements of national first-level reference material. GBW10010a has a total of 54 main trace elements. 39 elements have certified values and uncertainties and 15 elements only have reference values. The content of heavy metal elements such as As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Zn in GBW10010a decreased significantly, among which Cd, Cu, and Zn decreased by about 39%, 43% and 38.7%, respectively.
    CONCLUSIONSTo a certain extent, the values reflects the improvement of farmland ecological environment. Compared with the original GBW10010, the total number of certified value elements has increased by 6 items, including Ag and Nb (Nb gives reference values). Moreover, the uncertainty of each element is reduced, including biological-related elements Al, Cd, Cu, Fe, K, Mg, Mo, Na, P, Pb, Se, and Zn. The reduction indicates the technological advancement of the geological analysis and the improvement of the certified value level. In addition, the content of heavy metal elements in GBW10010a decreased significantly, reflecting the improvement of farmland ecological environment. The designated elements of the reference materials cover most of the main and trace elements with biological effects, and are suitable for the calibration of analytical instruments, evaluation of analytical methods, and monitoring analytical quality during agricultural ecological environment geochemical surveys and evaluation, biological sample analysis, agricultural product quality and food safety evaluation.

     

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