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电感耦合等离子体质谱法同时测定全血中锑、铋、锰和锌时的简化样品制备

Simplified sample preparation in the simultaneous measurement of whole blood antimony, bismuth, manganese, and zinc by inductively coupled plasma mass spectrometry.

作者信息

Haglock-Adler Carrie J, Strathmann Frederick G

机构信息

ARUP Institute for Clinical and Experimental Pathology, ARUP Laboratories, Salt Lake City, UT 84108, USA.

ARUP Institute for Clinical and Experimental Pathology, ARUP Laboratories, Salt Lake City, UT 84108, USA; University of Utah School of Medicine, Salt Lake City, UT 84108, USA.

出版信息

Clin Biochem. 2015 Feb;48(3):135-9. doi: 10.1016/j.clinbiochem.2014.11.012. Epub 2014 Nov 20.

DOI:10.1016/j.clinbiochem.2014.11.012
PMID:25448028
Abstract

OBJECTIVES

We developed and validated a simplified sample preparation for the analysis of antimony (Sb), bismuth (Bi), manganese (Mn), and zinc (Zn) in whole blood. This simplification included a reduction in sample volume, removal of a lengthy acidic digestion, and optimization of the internal standard.

DESIGN AND METHODS

Measurement of Sb, Bi, Mn and Zn in whole blood was conducted using inductively coupled-plasma mass spectrometry. Method performance characteristics, including intra- and inter-assay imprecision, accuracy, linearity, AMR, sensitivity, carryover, sample stability and assay stability were determined in accordance with clinical laboratory standards. In addition, analytical and clinical recoveries were assessed to investigate comparability between goat blood matrix and pooled patient blood.

RESULTS

Established assay performance characteristics included inter- and intra-assay imprecision <4.5% and carryover of <0.04% for all four elements, analytical measurement range of 1 to 25 μg/L (Sb and Bi), 1 to 80 μg/L (Mn), and 50 to 1500 μg/dL (Zn), limit of quantification of 1 μg/L (Sb, Bi, Mn) and 50 μg/dL (Zn) (coefficient of variation <14%), proportional bias of 0.96 and constant bias of -0.28 (Sb), 0.94 and -0.45 (Bi), 1.07 and -0.37 (Mn) and 0.96 and +18.05 (Zn) based upon repeat patient samples, proficiency testing samples, and comparison to an outside reference laboratory.

CONCLUSION

This method overcomes the laborious acidic heat digestion previously used and replaces it with a simplified sample preparation involving an alkaline dilution. The method requires minimal sample preparation with the dilution of alkaline diluent and is validated to quantify Sb and Bi from 1 to 25 μg/L, Mn from 1 to 80 μg/L, and Zn from 50 to 1500 μg/dL in whole blood.

摘要

目的

我们开发并验证了一种简化的样品制备方法,用于分析全血中的锑(Sb)、铋(Bi)、锰(Mn)和锌(Zn)。这种简化包括减少样品体积、去除冗长的酸性消解步骤以及优化内标。

设计与方法

使用电感耦合等离子体质谱法测定全血中的Sb、Bi、Mn和Zn。根据临床实验室标准确定方法性能特征,包括批内和批间不精密度、准确度、线性、分析测量范围、灵敏度、残留、样品稳定性和测定稳定性。此外,评估分析回收率和临床回收率,以研究山羊血基质与混合患者血液之间的可比性。

结果

既定的测定性能特征包括所有四种元素的批内和批间不精密度<4.5%,残留<0.04%,分析测量范围为1至25μg/L(Sb和Bi)、1至80μg/L(Mn)以及50至1500μg/dL(Zn),定量限为1μg/L(Sb、Bi、Mn)和50μg/dL(Zn)(变异系数<14%),基于重复患者样品、能力验证样品并与外部参考实验室比较,Sb的比例偏差为0.96,恒定偏差为-0.28;Bi的比例偏差为0.94,恒定偏差为-0.45;Mn的比例偏差为1.07,恒定偏差为-0.37;Zn的比例偏差为0.96,恒定偏差为+18.05。

结论

该方法克服了先前使用的繁琐酸性热消解方法,代之以一种涉及碱性稀释的简化样品制备方法。该方法只需用碱性稀释剂进行稀释,样品制备过程简单,并且经过验证可定量全血中1至25μg/L的Sb和Bi、1至80μg/L的Mn以及50至1500μg/dL的Zn。

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