牛血铅成分分析标准物质的研制

目的 研制牛血铅成分分析国家一级标准物质.方法 根据<一级标准物质技术规范(JJG1006-1994)>和ISO 17511要求,按照剂量.效应关系,选择2头雄性健康牛,以醋酸铅为饲料添加物,按每天2～5 mg/ks体重剂量喂养,制作牛血铅模型.当牛血铅分别达到90～100、190～200、280～300μg/L时,采集牛血,分装于密封性良好的耐低温管中,辐射后冷冻保存.进行均匀性检验、稳定性监测及放置室温时间检验.选用核素稀释质谱法(isotopic dilution mass spectrometry,ID-MS)为研制物质铅含量赋值.通过对美国NIST SRM 955b两个浓度样品铅含量的表达验证赋值方法.结果 铅含量分别为90～100、190～200、280～300 μg/L的低、中、高浓度组研制物质均匀性单因素方差分析F值分别为0.61、1.64、0.28,P值均大于0.05,说明3组研制物质均匀.经过14个月监测,3组浓度相对标准偏差分别为0.85%、1.05%和0.49%;与14个月前比较,t值分别为0.787、1.132、0.854,P值均大于0.05,表明研制物质14个月时间数值稳定.3组牛血铅的特性量值±不确定度分别为(102.4±5.5)、(181.2±4.0)、(304.5±3.9)μg/L.通过对美国NIST SRM 955b两个浓度样品铅含量的准确重现,说明赋值方法和程序正确.置常温下4 d内测定,结果稳定.结论 该络合型牛血铅成分分析研制物质的各项指标均达到国家一级标准物质的要求.

Development of bovine blood lead component analysis standard reference materials

Objective To develop the first grade standard analytical reference material of bovine blood lead.Methods According to standards and technology specification of primary standard reference material(JJGl006.1994),ISO 17511,and vollime.effect relationship,a bovine blood lcad model Was developed by adding acetate leed in the feed in dose of 2-5 mg·kg-1·d-1.Cow blcod was collected hen blood lead concentration went up to low,medium and high concentration range(90.100,190.200,280-300μg/L).Blood sample was kept in tube and frozen after irriadtion The samples were tested for homogeneity and stability.ID.MS method waft used to mea$ure the lcad concentration through comparison with two standard lead samples from the USA NIST SRM 955b.Results Samples of the three lead concentrations showed uniformity by single factor analysis of variance(F=0.61,1.64,0.28,respectively,P>0.05).After 14 months monitoring.the RSD was 0.85%.1.05%and 0.49%(t=0.787.1.132,0.854,respectively.P>0.05).The characteristic and indefinite values were 102.4 4-5.5:181.2±4.0;304.5± 3.9,respectively(unit:μg/L).,ne reproduction of the two USA NIST SRM 955b samples further showed our methods and procedures were correct.Our sample was stabile for four days at room temperature.C0ndusion The standard reference material of bovine in our research had reached the national standard material requirements.