Zearalenone (ZEN) is one of the most prevalent mycotoxins in corn and its products, which can accumulate in corn steep liquor (CSL) with much higher concentration after deep processing. For ensuring the precision of ZEN analysis in food safety, ZEN standard substance is critical. However, the preparation of standard substance usually needs complex chemical synthesis steps and large amounts of organic solvents consumption. Herein, a facile approach to extract ZEN from CSL for raw material of standard substance using polyamide 66 (PA) membrane as an adsorbent was proposed. Considering the coexistence of aflatoxin B