Abstract: A liquid chromatography-Orbitrap high resolution mass spectrometry (LC-HRMS) method and a TraceFinder database were developed for the screening and identification of 15 adulterated weight loss compounds in dietary supplements. The samples were extracted with methanol and filtered through a 0.22 μm microfiltration membrane prior to LC-HRMS analysis. The Full MS/dd-MS² mode was utilized in both positive and negative ion modes and the collected data were imported into the TraceFinder screening software. The established compound database and screening method were used for rapid, automatic, and high-precision screening to determine if the weight loss compounds were adulterated. The method validation results indicated that all of the analytes showed excellent linear relationships with regression coefficients (r) above 0.998. The recoveries were in the range of 79.7%-95.4% while the precisions ranged from 3.3% to 8.7%. The method and database were used to screen weight loss adulterants in 29 batches of dietary supplements; six batches of samples tested positive for adulterants with the identification of four compounds including sibutramine. This method enables the automatic high-precision screening and identification of adulterants, providing a novel and powerful tool for combating the increasingly rampant occurrence of adulteration in dietary supplements.

Key words: adulteration, health food, high resolution mass spectrometry (HRMS), identification, liquid chromatography (LC), screening