윤새나 (식품의약품안전평가원 첨단분석과)

김현경 (식품의약품안전평가원 첨단분석과)

이현경 (식품)

윤새나 (식품의약품안전평가원 첨단분석과)

박보름 (식품의약품안전평가원)

김형수 (식품의약품안전평가원 첨단분석과)

김현경 (식품의약품안전평가원 첨단분석과)

The growing demand for anti-obesity products, along with the development of novel peptide-based therapeutics, has increased the need for analytical methods for regulatory surveillance of the manufacturing and distribution of illicit products. In this study, a simultaneous LC–MS/MS method was developed and validated for 12 peptide compounds associated with obesity treatment, including active ingredients of approved pharmaceutical products and compounds currently under development. The MRM transitions were established using multiply charged precursor ions and peptide-specific b- and y-ions. The chromatographic conditions were optimized to achieve adequate separation, good peak shape, and sufficient signal intensity for all analytes. The method showed excellent linearity within the individual calibration ranges of each analyte, with correlation coefficients(r²) exceeding 0.999. Recovery rates were evaluated between 84.93 to 113.93%, and matrix effects were also evaluated and showed acceptable variability, with CV values ≤ 15%. Intra-day precision and accuracy ranged from 0.60 to 13.87% and 82.47 to 113.62%, respectively, while inter-day precision and accuracy ranged from 1.04 to 14.10% and 85.01 to 106.99%, respectively. The established method was applied to commercially availabele injectable products containing liraglutide(Saxenda®, Xultophy®), semaglutide(Wegovy®, Ozempic®), tirzepatide(Mounjaro®), and lixisenatide(Soliqua®). The measured contents of the peptides in the respective products ranged from 94.83% to 108.60% of the labeled amount. These findings demonstrate that the method is suitable for rapid screening and confirmatory analysis of peptide-based pharmaceuticals and may help prevent illicit product distribution in the Korean market.

Acknowledgement: This research was supported by a grant(25211MFDS001) from Ministry of Food and Drug Safety in 2026.