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目的建立电感耦合等离子体-质谱(ICP-MS)法测定尿和全血中锗(Ge)的检测方法。方法尿样用体积分数为0.50%硝酸稀释10倍,血样用体积分数为0.10%聚乙二醇辛基苯基醚加体积分数为0.25%硝酸稀释10倍后直接用ICP-MS法测定,应用标准曲线法和内标校正法定量。结果 Ge在0.00~100.00μg/L线性良好,相关系数为1.000;尿Ge检出限为8.50×10-3μg/L,血Ge检出限为1.30×10-2μg/L;尿Ge加标回收率为95.87%~101.32%,批内精密度为0.56%~4.89%,批间精密度为1.11%~5.08%;血Ge加标回收率为94.30%~104.02%,批内精密度为0.92%~4.29%,批间精密度为2.36%~4.95%。结论本法灵敏度高、精密度好,结果准确可靠,适合尿和全血中Ge的测定。
Objective To establish a method for the determination of Ge in urine and whole blood by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Methods The urine samples were diluted 10 times with 0.50% nitric acid. The blood samples were determined by ICP-MS when 0.10% polyethylene glycol octylphenyl ether and 0.25% nitric acid were used as the volume fraction. Standard curve method and internal standard method for quantification. Results The calibration curve of Ge was linear in the range of 0.00-100.00μg / L with a correlation coefficient of 1.000. The detection limit of urine Ge was 8.50 × 10-3μg / L and the detection limit of blood Ge was 1.30 × 10-2μg / L. The intra-assay precision ranged from 95% to 101.32%, the intra-assay precision ranged from 0.56% to 4.89%, and the intra-assay precision ranged from 1.11% to 5.08%. The recovery rates of spiked blood Ge ranged from 94.30% to 104.02% ~ 4.29%, inter-batch precision of 2.36% ~ 4.95%. Conclusion This method has high sensitivity, good precision and accurate and reliable results. It is suitable for the determination of Ge in urine and whole blood.