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基于Sandell-Kolthoff 反应的微量板分光光度法测定唾液碘的介绍。

Introduction of a spectrophotometric method for salivary iodine determination on microplate based on Sandell-Kolthoff reaction.

机构信息

Division of Nuclear Medicine, University Medical Centre Ljubljana, Ljubljana, Slovenia.

Faculty of Medicine, University of Ljubljana, Ljubljana, Slovenia.

出版信息

Radiol Oncol. 2024 Jul 22;58(3):357-365. doi: 10.2478/raon-2024-0035. eCollection 2024 Sep 1.

Abstract

BACKGROUND

Iodine is an essential element for the synthesis of thyroid hormones. Therefore, a reliable marker of iodine supply is important. Iodine is predominantly excreted via kidneys, but also via salivary glands. Our aim was to introduce a new and simple method for determination of salivary iodine concentration (SLIC).

MATERIALS AND METHODS

Self-prepared chemicals and standards for Sandell-Kolthoff reaction on microplate with ammonium peroxydisulfate (AP) in the range 0-400 µg/L were used. Suitability of water-based standards (WBS) and artificial saliva-based standards (ASS) for standard curve were tested. We followed standards for method validation, defined concentration of used AP and compared our results with Inductively Coupled Plasma Mass Spectrometry (ICP-MS).

RESULTS

WBS gave more reliable results than ASS as an underestimation of iodine concentration was found for ASS. LoB was 6.5 µg/L, LoD 12.0 µg/L, therefore analytical range was 12-400 µg/L. Intra- and inter-assay imprecisions at iodine concentrations, namely 20, 100, 165, and 350 µg/L were 18.4, 5.1, 5.7, and 2.8%, respectively, and 20.7, 6.7, 5.1, and 4.3%, respectively. Suitable molarity of AP was 1.0 mol/L and showed no difference to 1.5 mol/L (P values for samples with concentration 40, 100, and 150 µg/L, were 0.761, 0.085, and 0.275, respectively), whereas there was a significant change using 0.5 mol/L (P<0.001). Saliva samples could be diluted up to 1:8. There was no interference of thiocyanate and caffeine up to 193.5 mg/L. Our original method was comparable to ICP-MS. Spaerman coefficient was 0.989 (95% CI: 0.984-0.993).

CONCLUSIONS

The new method for SLIC determination is in excellent agreement with ICP-MS and easy-to-use.

摘要

背景

碘是合成甲状腺激素的必需元素。因此,可靠的碘供应标志物非常重要。碘主要通过肾脏排泄,但也通过唾液腺排泄。我们的目的是引入一种新的、简单的唾液碘浓度(SLIC)测定方法。

材料和方法

使用自行制备的化学品和标准品,在微孔板上进行 Sandell-Kolthoff 反应,使用过硫酸铵(AP)的范围为 0-400 µg/L。测试了基于水的标准品(WBS)和基于人工唾液的标准品(ASS)用于标准曲线的适用性。我们遵循方法验证标准,定义了所用 AP 的浓度,并将结果与电感耦合等离子体质谱法(ICP-MS)进行了比较。

结果

WBS 比 ASS 更可靠,因为 ASS 会低估碘浓度。LoB 为 6.5 µg/L,LoD 为 12.0 µg/L,因此分析范围为 12-400 µg/L。在碘浓度分别为 20、100、165 和 350 µg/L 时,日内和日间精密度分别为 18.4%、5.1%、5.7%和 2.8%,以及 20.7%、6.7%、5.1%和 4.3%。合适的过硫酸铵浓度为 1.0 mol/L,与 1.5 mol/L 无差异(浓度为 40、100 和 150 µg/L 的样品的 P 值分别为 0.761、0.085 和 0.275),而使用 0.5 mol/L 时则有显著变化(P<0.001)。唾液样本可稀释至 1:8。硫氰酸盐和咖啡因高达 193.5 mg/L 时无干扰。我们的原始方法与 ICP-MS 相当。Spearman 系数为 0.989(95%CI:0.984-0.993)。

结论

新的 SLIC 测定方法与 ICP-MS 非常吻合,易于使用。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/27fc/11406899/700558e9f978/j_raon-2024-0035_fig_001.jpg

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