Supramolecular Solvent-Based Extraction of Bisphenols and Alkylphenols in Botanical Dietary Supplements Prior to HPLC–MS/MS Analysis

Dietary supplements provide essential nutrients and bioactive compounds that enhance health and traditional therapies. However, the quality and composition of these supplements can vary significantly, potentially containing inconsistent levels of active ingredients or undisclosed risk substances. Due to the current extensive industrial applications, bisphenols (BPs) and alkylphenols (APs) have become environmentally ubiquitous. Substantial evidence indicates that these compounds exhibit endocrine-disrupting properties, posing potential health risks to humans. The detection of trace-level BPs and APs in dietary supplements is critical. This study developed a supramolecular solvent (SUPRAS) from a water/THF/1-hexanol system under mild conditions for analyzing 19 BPs and APs in commercial botanical dietary supplements. After optimizing SUPRAS preparation and extraction parameters, we established a SUPRAS-HPLC-MS/MS method enabling one-step extraction/cleanup within 10 min for tablets, capsules, and oral liquids, with high sensitivity and simplicity. The method scored 0.71 (out of 1) on the AGREE metric, confirming its green profile. Detectable levels of bisphenol A (178.7-452.6 μg/kg) and 4-pentylphenol (145.3 μg/kg) in marketed products highlight potential health risks from botanical dietary supplement-derived exposure.