Meldonium determination in milk and meat through UHPLC-HRMS

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Abstract

A simple and sensitive procedure for the quantification of meldonium in milk and meat by UHPLC-HRMS is presented. Some products were investigated to contain this substance due to using a veterinary drug called “Emidonol”. According to the instruction for this drug, it can be used for injection (for cows) and as an additive in drinking water for chickens. Although meldonium is not a threat for human health, it is strictly prohibited in professional sports according to WADA Prohibited List. Sample preparation conditions were optimized for both matrices that allowed to eliminate matrix effects and achieve reproducible and accurate results. Protein precipitation with dilution were applied for milk samples, while chicken meat and liver were homogenized with quartz sand to achieve satisfactory meldonium recovery. The results of milk and meat samples analysis purchased at the farmers’ fair are presented in this article. Meldonium concentration in raw milk was investigated to be up to 880 ng/mL. However, pasteurization can be used for partial cleanup from meldonium (up to 2 times). The same research was conducted for chicken meat and liver. Thermal treatment shows a good result for a meat cleanup. The proposed method was partially validated, limits of detection and quantification were established for each matrix.

Abstract

Analytical chemistry; Food Analysis, meldonium; UHPLC-HRMS; milk; Meat; liver; doping; Food Safety; quantification; Emidonol

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Is Open Access

Mildronate (Meldonium) in professional sports – monitoring doping control urine samples using hydrophilic interaction liquid chromatography – high resolution/high accuracy mass spectrometry

Christian Görgens, Sven Guddat, Josef Dib … (2015)

To date, substances such as Mildronate (Meldonium) are not on the radar of anti‐doping laboratories as the compound is not explicitly classified as prohibited. However, the anti‐ischemic drug Mildronate demonstrates an increase in endurance performance of athletes, improved rehabilitation after exercise, protection against stress, and enhanced activations of central nervous system (CNS) functions. In the present study, the existing evidence of Mildronate's usage in sport, which is arguably not (exclusively) based on medicinal reasons, is corroborated by unequivocal analytical data allowing the estimation of the prevalence and extent of misuse in professional sports. Such data are vital to support decision‐making processes, particularly regarding the ban on drugs in sport. Due to the growing body of evidence (black market products and athlete statements) concerning its misuse in sport, adequate test methods for the reliable identification of Mildronate are required, especially since the substance has been added to the 2015 World Anti‐Doping Agency (WADA) monitoring program. In the present study, two approaches were established using an in‐house synthesized labelled internal standard (Mildronate‐D3). One aimed at the implementation of the analyte into routine doping control screening methods to enable its monitoring at the lowest possible additional workload for the laboratory, and another that is appropriate for the peculiar specifics of the analyte, allowing the unequivocal confirmation of findings using hydrophilic interaction liquid chromatography‐high resolution/high accuracy mass spectrometry (HILIC‐HRMS). Here, according to applicable regulations in sports drug testing, a full qualitative validation was conducted. The assay demonstrated good specificity, robustness (rRT=0.3%), precision (intra‐day: 7.0–8.4%; inter‐day: 9.9–12.9%), excellent linearity (R>0.99) and an adequate lower limit of detection (<10 ng/mL). © 2015 The Authors. Drug Testing and Analysis published by John Wiley & Sons, Ltd.