In this study, gold nanoparticles (AuNPs) modified with β-cyclodextrin (β-CD) were used to assist with electromembrane extraction (EME) and were coupled with capillary electrophoresis (CE) and ultraviolet (UV) detection (CE-UV) for the extraction and measurement of methadone from plasma samples. A β-CD-modified AuNP-reinforced hollow fiber (HF) was utilized in this work. The β-CD-modified AuNPs act as an absorbent and provide an extra pathway for the analyte extraction. For obtaining the effect of the presence of β-CD-modified AuNPs in the HF pores, the extraction efficiency of the EME and β-CD-modified AuNPs/EME techniques were compared. Different parameters influencing the extraction efficacy of the EME and β-CD-modified AuNPs/EME methods were optimized. Optimal extractions were performed with 1-octanol as the organic solvent in the supported liquid membrane (SLM), with an applied voltage of 10 V as the driving force across the SLM, and with pH 7.0 in the donor solutions with a stirring speed of 1000 rpm after 20 min and 25 min for the β-CD-modified AuNPs/EME and EME methods, respectively. Under optimal conditions, compared with the EME method, the β-CD-modified AuNPs/EME method exhibited increased extraction efficacy in a short time. The β-CD-modified AuNPs/EME technique demonstrated a lower limit of detection (5.0 ng mL-1), higher extraction recovery (68%), and a more optimal preconcentration factor (135). Furthermore, this method was successfully utilized for measuring methadone in real plasma samples.
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