Multi-Metric Assessment of Liquid Chromatography–Mass Spectrometry Methods for Mycotoxin Determination in Human Urine: Advancing Sustainable, Practical, and Innovative Analytical Practices

Background/Objectives: Human biomonitoring of mycotoxins is important for assessing exposure and its associated health risks. Modern analytical chemistry aims to enhance sustainability, practicality, and modernization of analytical methods. Therefore, developing sensitive, selective, cost-effective, and environmentally friendly methods is highly desirable. This study aimed at evaluating liquid chromatographic methods reported for the determination of mycotoxins in human urine, identifying their strengths, limitations, and future development needs and providing guidance for selecting the most appropriate methods. Methods: Twelve liquid chromatographic methods for mycotoxin determination in urine were selected. The methods were evaluated in terms of environmental sustainability, practical applicability, and innovation. Five complementary metrics, namely the Analytical GREEnness Metric, Modified Green Analytical Procedure Index, Click Analytical Chemistry Index, Blue Applicability Grade Index, and Innovative Method Orange Gradient Index, were utilized. Results: Most of the evaluated methods exhibited acceptable levels of eco-friendliness and moderate to good practical applicability, but limited innovation. Within the scope of the selected multi-criteria assessment framework, method 5 achieved the highest overall score owing to its multianalyte capability, efficient sample preparation, reduced sample and solvent consumption, and favorable sustainability, practicality, and innovation characteristics. Conclusions: The findings highlight the need for more practical and technologically advanced analytical methods that align with the principles of green and modern analytical chemistry principles, thereby supporting more sustainable and efficient biomonitoring of mycotoxins.