Dyke Jason V, Dasgupta Purnendu K, Kirk Andrea B
Department of Chemistry and Biochemistry, Texas Tech University, Lubbock, TX 79409-1061, USA.
Talanta. 2009 Jul 15;79(2):235-42. doi: 10.1016/j.talanta.2009.03.038. Epub 2009 Mar 26.
Accurate quantitation of iodine in biological samples is essential for studies of nutrition and medicine, as well as for epidemiological studies for monitoring intake of this essential nutrient. Despite the importance of accurate measurement, a standardized method for iodine analysis of biological samples is yet to be established. We have evaluated the effectiveness of (72)Ge, (115)In, and (129)I as internal standards for measurement of iodine in milk and urine samples by induction coupled plasma mass spectrometry (ICP-MS) and of (35)Cl(18)O(4)(-), (129)I(-), and 2-chlorobenzenesulfonate (2-CBS) as internal standards for ion chromatography-tandem mass spectrometry (IC-MS/MS). We found recovery of iodine to be markedly low when IC-MS/MS was used without an internal standard. Percent recovery was similarly low using (35)Cl(18)O(4) as an internal standard for milk and unpredictable when used for urine. 2-Chlorobenzebenzenesulfonate provided accurate recovery of iodine from milk, but overestimated iodine in urine samples by as much as a factor of 2. Percent recovery of iodine from milk and urine using ICP-MS without an internal standard was approximately 120%. Use of (115)In predicted approximately 60% of known values for both milk and urine samples. (72)Ge provided reasonable and consistent percent recovery for iodine in milk samples (approximately 108%) but resulted in approximately 80% recovery of iodine from urine. Use of (129)I as an internal standard resulted in excellent recovery of iodine from both milk and urine samples using either IC-MS/MS and ICP-MS.
准确定量生物样品中的碘对于营养和医学研究以及监测这种必需营养素摄入量的流行病学研究至关重要。尽管准确测量很重要,但生物样品碘分析的标准化方法尚未建立。我们评估了(72)Ge、(115)In和(129)I作为电感耦合等离子体质谱(ICP-MS)测定牛奶和尿液样品中碘的内标,以及(35)Cl(18)O(4)-、(129)I-和2-氯苯磺酸盐(2-CBS)作为离子色谱-串联质谱(IC-MS/MS)内标的有效性。我们发现,在没有内标的情况下使用IC-MS/MS时,碘的回收率明显较低。使用(35)Cl(18)O(4)作为牛奶的内标时,回收率同样较低,而用于尿液时则不可预测。2-氯苯磺酸盐能准确回收牛奶中的碘,但将尿液样品中的碘高估了多达2倍。在没有内标的情况下,使用ICP-MS从牛奶和尿液中回收碘的百分比约为120%。使用(115)In预测牛奶和尿液样品的已知值约为60%。(72)Ge为牛奶样品中的碘提供了合理且一致的回收率(约108%),但从尿液中回收碘的回收率约为80%。使用(129)I作为内标,无论是使用IC-MS/MS还是ICP-MS,都能从牛奶和尿液样品中出色地回收碘。