直接稀释-石墨炉原子吸收法快速批量测定人尿中的铅
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摘要
目的建立石墨炉原子吸收标准加入校准法快速批量测定人尿中铅的方法。方法取尿样0.20 ml用稀释液直接稀释5倍,氯化钯作基体改进剂,塞曼扣除背景,标准加入校准法,峰面积定量,直接自动测定。结果方法的线性范围0μg/L~80.0μg/L,线性相关系数为0.9995,方法的最低检出限为1.0μg/L,相对标准偏差(RSD)为3.4%~6.2%,加标回收率为95%~102%,应用本法测定冻干人尿中铅标准物质GBW09104f/09105f,结果均在标准值的允许误差范围内。结论本法标准曲线与样品的基体更为一致,精密度、准确度良好,自动化程度高。是一种简便、快速、适合批量尿铅测定的方法。
Objective To develop a rapid method for determination of urine plumbum by GFAAS and standard addition calibration.Methods Urine sample(0.20 ml) was diluted 5 times with 1 ml / L nitrate and 0.1 g / L TritonX-100,and directly determined by GFAAS,with PdCl 2 as matrix modifier,peak area for quantification and standard addition calibration.Results The significant linear relation between absorbance and Lead level was 0 μg / L ~ 80.0 μg / L,the correlation coefficient was 0.9995,the lowest detection limit was 1.0 μg / L,the RSD of parallel double sample was 3.4% ~ 6.2%,the recovery of standard addition was 95% ~ 102%.The method was successfully applied to determine Certified Reference Materials such as GBW09104f /09105f,and the results were in good agreement with the certified values.Conclusion The measurement is characterized by high accuracy and precision,a high degree of automation,so the method is good for determination of urine plumbum rapidly in batch.
Objective To develop a rapid method for determination of urine plumbum by GFAAS and standard addition calibration.Methods Urine sample(0.20 ml) was diluted 5 times with 1 ml / L nitrate and 0.1 g / L TritonX-100,and directly determined by GFAAS,with PdCl 2 as matrix modifier,peak area for quantification and standard addition calibration.Results The significant linear relation between absorbance and Lead level was 0 μg / L ~ 80.0 μg / L,the correlation coefficient was 0.9995,the lowest detection limit was 1.0 μg / L,the RSD of parallel double sample was 3.4% ~ 6.2%,the recovery of standard addition was 95% ~ 102%.The method was successfully applied to determine Certified Reference Materials such as GBW09104f /09105f,and the results were in good agreement with the certified values.Conclusion The measurement is characterized by high accuracy and precision,a high degree of automation,so the method is good for determination of urine plumbum rapidly in batch.
引文
[1]李春玲.尿中铅、镉石墨炉原子吸收光谱测定方法[J].卫生研究,2002,31(4):303-304.
[2]WS/T 18-1996.尿中铅的石墨炉原子吸收光谱测定方法[S].
[3]许兵,康正利.石墨炉原子吸收法直接测定尿中的铅[J].中国卫生检验杂志,2010,20(7):1653-1655.
[4]包青峰,段妮.石墨炉标准加入校正法快速批量测定全血中铅[J].中国卫生检验杂志,2008,18(12):2595-2596.
[5]李拥军,孙建云.石墨炉原子吸收光谱法测定尿样中铅[J].理化检验-化学分册,2008,44(4):357-358.
[6]荀晔.氯化钯作改进剂石墨炉原子吸收法测定尿中铅[J].检验医学与临床,2012,9(1):84-85.
[2]WS/T 18-1996.尿中铅的石墨炉原子吸收光谱测定方法[S].
[3]许兵,康正利.石墨炉原子吸收法直接测定尿中的铅[J].中国卫生检验杂志,2010,20(7):1653-1655.
[4]包青峰,段妮.石墨炉标准加入校正法快速批量测定全血中铅[J].中国卫生检验杂志,2008,18(12):2595-2596.
[5]李拥军,孙建云.石墨炉原子吸收光谱法测定尿样中铅[J].理化检验-化学分册,2008,44(4):357-358.
[6]荀晔.氯化钯作改进剂石墨炉原子吸收法测定尿中铅[J].检验医学与临床,2012,9(1):84-85.