圆白菜、菠菜成分分析国家一级标准物质复研制  

Replication of Cabbage and Spinach Certified Reference Materials for Biochemical Analysis

作　　者：赵凯 潘含江[1] 杨榕[1] 刘妹[1] 周国华[1] 顾雪 徐进力[1] ZHAO Kai;PAN Hanjiang;YANG Rong;LIU Mei;ZHOU Guohua;GU Xue;XU Jinli(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang,Hebei 065000,China)

机构地区：[1]中国地质科学院地球物理地球化学勘查研究所,河北廊坊065000

出　　处：《中国无机分析化学》2024年第9期1331-1339,共9页Chinese Journal of Inorganic Analytical Chemistry

基　　金：中央级公益性科研院所基本科研业务费项目(ZY202001);中国地质科学院地球物理地球化学勘查研究所科研项目(ZY202001)。

摘　　要：为了满足农产品分析测试的需求,提升农业领域元素检测能力,开展对国家一级标准物质圆白菜GBW10014、菠菜GBW10015的复研制工作。在样品原采集地采集样品,经粗碎、干燥、细碎、过筛、混匀,分装于高密度聚乙烯塑料瓶(25 g/瓶),经钴-60辐照灭活后,4~8℃长期储存。针对30余种代表性成分进行了均匀性检验,并在1 a内分5个时间点对32种易变、有代表性成分开展长期稳定性检验,主要采用电感耦合等离子体光谱法(ICP-OES)、电感耦合等离子体质谱法(ICP-MS)测试,结果表明样品均匀性、稳定性良好。选择11家实验室采用多种方法对60种成分进行合作定值,建立了合理的量值溯源链。数据经可疑值检验与剔除、正态分布检验后,采用算数平均值作为认定值。对不确定度进行了详细评定,最终合成不确定度中包括定值过程、均匀性及稳定性引入的不确定度。圆白菜定值56种成分,菠菜定值58种成分,大部分成分含量与原批次相当,认定值数量均多于原批次,且不确定度水平有所提高。复研制过程符合规范要求,经审查获得国家一级标准物质证书。In order to meet the needs of agricultural product analysis and improve the ability of element detection in the agricultural field,the replication of two national first-class certified reference materials,cabbage powder GBW10014 and spinach powder GBW10015,had been carried out.The samples were collected from the original collection sites,and then packed with 25 g in each high-density polyethylene plastic bottle after they were prepared by coarse crushing,drying,fine crushing,sifting and mixing.After being inactivated by 60 Co,the samples were stored at 4—8℃for a long time.The homogeneity test of more than 30 representative components was conducted,and the long-term stability test of 32 volatile and representative components was carried out at 5 time points in one year.The samples were mainly determined by inductively coupled plasma spectrometry(ICP-OES)and inductively coupled plasma mass spectrometry(ICP-MS).The results showed that the sample homogeneity and stability were fairly good.A total of 11 laboratories were selected to implement sample analysis.A reasonable quantity traceability chain was established.Various methods were used to determine the value of 60 components.After suspicious value test and elimination,normal distribution test,arithmetic mean value was used as the certified value.The uncertainty was evaluated in detail,and the final synthetic uncertainty included the uncertainty introduced by the analysis process,homogeneity and stability.56 elements in Chinese cabbage powder and 58 elements in spinach powder were determined,and most of the elements concentrations were the comparable to those in the original batch.The number of certified values was more than that in the original batch,and the uncertainty level was increased.The replication process meets the requirements of the standard,and the national first-class standard material certificate is obtained after examination.

关 键 词：圆白菜 菠菜 国家一级标准物质 稳定性 均匀性 定值 

分 类 号：O657.31[理学—分析化学] O657.63[理学—化学]