血清中碘的测定:电感耦合等离子体-质谱法的验证
Determination of iodine in serum: verification of inductively coupled plasma mass spectrometry
摘要目的:验证电感耦合等离子体-质谱法(ICP-MS)对血清中碘含量的测定,并评价ICP-MS法与砷铈催化分光光度法测定血清碘的一致性。方法:采用ICP-MS法测定血清中的碘含量,以铼( 187Re)作为内标,优化各项参数;采用ICP-MS法和砷铈催化分光光度法同时测定88份血清样本,方法学评价指标包括标准曲线的测定范围、最低检出限、精密度、准确度。并且通过组间相关分析、组内相关系数(ICC)分析、Passing-Bablok回归和Bland-Altman偏差图分析评价两种方法的一致性。 结果:ICP-MS方法标准曲线的线性范围为0 ~ 300 μg/L,碘浓度值与碘响应值之间呈现良好的线性相关关系,相关系数范围为0.999 8 ~ 0.999 9;最低检出限为1.96 μg/L;血清样测定的批内和批间精密度实验的相对标准偏差( RSD)范围分别为0.2% ~ 1.4%、0.4% ~ 1.8%;加标回收率范围为90.44% ~ 108.71%。88份血清样相关分析的结果显示,两种方法测定结果显著相关( r = 0.934, P < 0.05);ICC为0.932;Passing-Bablok回归结果显示,两种方法的偏倚差异无统计学意义( P > 0.05);Bland-Altman图提示两种方法的测定结果具有一致性。 结论:ICP-MS测定方法最低检出限低,精密度和准确度高,简便快速且易于操作,适用于大批量血清样本中碘含量的检测;ICP-MS法与砷铈催化分光光度法测定血清碘结果具有一致性。
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abstractsObjective:To verify the determination method of iodine in serum by inductively coupled plasma mass spectrometry (ICP-MS) and to evaluate the consistency between ICP-MS and As 3+-Ce 4+ catalytic spectrophotometry in determination of serum iodine. Methods:Serum iodine concentration was determined by ICP-MS, 187Re was used as an internal standard, and ralated parameters were optimized. Eighty-eight serum samples were simultaneously determined by ICP-MS and As 3+-Ce 4+ catalytic spectrophotometry, and the evaluation indexes included determination range of standard curve, detection limit, precision, accuracy. In addition, we also evaluated the consistency of the two methods through inter-group correlation analysis, intra-group correlation coefficient analysis, Passing-Bablok regression and Bland-Altman analysis. Results:The linear range of ICP-MS standard curve was 0 - 300 μg/L. There was a good linear correlation between iodine concentration value and iodine response value, and the correlation coefficient range was 0.999 8 to 0.999 9. The detection limit of the ICP-MS method was 1.96 μg/L. The relative standard deviation ( RSD) ranged from 0.2% to 1.4% and from 0.4% to 1.8% for intra and inter-batch precision tests of serum samples. The recovery rate ranged from 90.44% to 108.71%. The correlation analysis of 88 serum samples showed that there was a good correlation between the two methods ( r = 0.934, P < 0.05), and the intra-class correlation coefficient was 0.932. The results of Passing-Bablok regression showed that there was no significant difference between the two methods ( P > 0.05). Bland-Altman diagram suggested that the results of the two methods were consistent. Conclusions:ICP-MS method has low detection limit, high precision and accuracy. ICP-MS method is simple, rapid, easy and suitable for determination of iodine in large quantities of serum samples. The results of the two methods for determining serum iodine are consistent.
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