Analysis of Hypoxia-Inducible Factor Stabilizers by a Modified QuEChERS Extraction for Antidoping Analysis

IF 0.4 Q4 SPECTROSCOPY

Mass Spectrometry Letters Pub Date : 2020-01-01 DOI:10.5478/MSL.2020.11.4.118

S. Kim, Nu Ri Lim, H. Min, Changmin Sung, H. Oh, Ki Hun Kim

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引用次数: 2

Abstract

An analytical method was developed for hypoxia-inducible factor (HIF) stabilizers based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) sample preparation and liquid chromatography-high resolution mass spectrometry analysis. HIF stabilizers potentially enhance the performance of athletes, and hence, they have been prohibited. However, the analysis of urinary HIF stabilizers is not easy owing to their unique structure and characteristics. Hence, we developed the QuEChERS preparation technique for a complementary method and optimized the pH, volume of extraction solvent, and number of extractions. We found that double extraction with 1% of formic acid in acetonitrile provided the highest recovery of HIF stabilizers. Moreover, the composition of the mobile phase was also optimized for better separation of molidustat and IOX4. The developed method was validated in terms of its precision, detection limit, matrix effect, and recovery for ISO accreditation. To the best of our knowledge, this is the first demonstration of the application of the QuEChERS method, which is suitable as a complementary analytical method, in antidoping.

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用改良的QuEChERS萃取法分析缺氧诱导因子稳定剂的反兴奋剂分析

建立了一种基于QuEChERS(快速、简便、廉价、有效、坚固、安全)样品制备和液相色谱-高分辨质谱分析的低氧诱导因子(HIF)稳定剂分析方法。HIF稳定剂可能会提高运动员的表现，因此，它们被禁止使用。然而，由于其独特的结构和特性，分析尿HIF稳定剂并不容易。因此，我们开发了QuEChERS制备技术作为补充方法，并优化了提取溶剂的pH、体积和提取次数。结果表明，在乙腈中以1%甲酸进行二次萃取时，HIF稳定剂的回收率最高。此外，还对流动相的组成进行了优化，以更好地分离莫里司他和IOX4。对该方法的精密度、检出限、基质效应和回收率进行了验证。据我们所知，这是QuEChERS方法的第一次应用演示，它适合作为一种补充分析方法，用于反兴奋剂。

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