Development of an MSPE-UHPLC-MS/MS method for bisphenols and alkylphenols in personal care products: a pilot study...

As daily essentials for skin protection and cosmetic enhancement, personal care products (PCPs) are used extensively worldwide. Due to their direct and prolonged contact with the skin, any hazardous ingredients they contain warrant serious attention. Although bisphenols (BPs) and alkylphenols (APs) are of growing concern for their known or potential endocrine-disrupting effects, most research has targeted food, water, and environmental samples, with comparatively few methods available for their analysis in PCPs. To assess the occurrence and potential risks of such substances in PCPs, this study established a corresponding detection method and performed a preliminary safety evaluation. The diversity and compositional complexity of PCPs complicate the detection of BPs and APs at trace levels. Therefore, a broadly applicable and reliable analytical method was developed and validated based on magnetic solid-phase extraction (MSPE) coupled with isotope-labeled internal standards (IL-ISs) and ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Sample pretreatment conditions, as well as chromatographic and mass spectrometric parameters, were systematically investigated. During the MSPE process, the Fe₃O₄@HLB magnetic material was employed for sample pretreatment, providing straightforward operation and effective sample purification coupled with analyte enrichment. The established method satisfied the requirements for qualitative and quantitative analysis of 23 BPs and APs in various PCP matrices, and was further applied to the analysis of PCPs sold in China. Five substances including bisphenol A (BPA) and bisphenol F (BPF) were detected at concentrations ranging from 5.5 to 226.5 µg kg^-1. Based on the measured concentrations, a preliminary safety evaluation of the potential health risks associated with residual BPF in children's PCPs was conducted by calculating the margin of safety (MoS). The developed MSPE-UHPLC-MS/MS method with IL-ISs in this study proved to be convenient, efficient, and feasible for the determination of trace contaminants in PCPs. This work not only provides preliminary occurrence and risk-assessment data on APs and BPs in PCPs sold in China but also provides the technical basis and baseline data necessary to inform the development of regulatory policies.