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建立离子色谱-电感耦合等离子体质谱(IC-ICP-MS)联用测定人尿中碘和钼形态的方法,该方法对IO3-和I-检出限分别为0.1 ng/mL和0.2 ng/mL,对MoO42-(以Mo计)的检出限为0.4 ng/mL,IO3-(以I计)、I-和MoO42-(以Mo计)线性回归系数r均大于0.999。检测实际尿样中I-和MoO42-(以Mo计)相对标准偏差RSD均小于5%,实际尿样中未发现IO3-。尿样中I-和MoO42-(以Mo计)的加标回收试验表明其回收率在91%～102%之间。本文利用尺寸排阻色谱-电感耦合等离子体质谱(SEC-ICP-MS)联用首次直接证明人尿中还存在至少3种形态有机碘以及1种形态有机钼。
A method for the determination of iodine and molybdenum in human urine by ion chromatography-inductively-coupled plasma mass spectrometry (IC-ICP-MS) was developed. The detection limits of IO3- and I- were 0.1 ng / mL and 0.2 ng / mL, and the detection limits for MoO42- (Mo) were 0.4 ng / mL, IO3- (calculated as I), linear regression coefficients r of I- and MoO42- (calculated as Mo) were all greater than 0.999. The relative standard deviations (RSDs) of both I- and MoO42- (calculated as Mo) in real urine samples were all less than 5%. No actual IO3- was found in urine samples. The spiked recoveries of I- and MoO42- (calculated as Mo) in urine samples showed recoveries between 91% and 102%. In this paper, the first direct evidence of the existence of at least three kinds of organic iodine and one kind of organic molybdenum in human urine by size-exclusion chromatography-inductively coupled plasma mass spectrometry (SEC-ICP-MS)