NMR Analysis of Pulegone in Food Products

Abstract

Featured Application: This NMR-based analytical method for pulegone detection could help food safety laboratories rapidly screen mint-flavored products and essential oils for compliance with regulatory limits. The approach is particularly valuable for quality control in the food and flavoring industry, where fast and reliable pulegone quantification is essential to ensure consumer safety, especially given pulegone’s classification as a possible human carcinogen. Pulegone is a monoterpene ketone found in a variety of mint species. It has been classified as possibly carcinogenic to humans (Group 2B) by the International Agency for Research on Cancer (IARC). In previous studies, pulegone in food was analyzed exclusively via GC-MS, while 1H NMR methods were limited to essential oils. The aim of this study was to develop an NMR method for the detection and quantification of pulegone in essential oils and foods. A mixture of methanol-d4/chloroform-d1 in a 1:1 ratio (v/v) was identified as the most effective solvent for separating pulegone signals. The essential oils were subjected to analysis at this solvent-mixture ratio. The extraction of pulegone was required for food analysis, and the steam distillation method proved to be more effective than the ultrasonic-assisted extraction method. The highest pulegone concentrations were identified in pennyroyal oil and muña oil, whereas lower levels were observed in other matrices, including corn mint oil and select food items. A toxicological assessment showed that the amount consumed did not exert any adverse effects on human health.