The present study explains the in-situ growth of Co-Al layered double hydroxide coated on the anodized aluminum substrate for thin film microextraction (TFME) approach. Anodizing process was performed by applying electrochemical (chronoamperometry) method on a cost-effective Al foil as substrate. Multivariate optimization method has been explored for TFME of quercetin from different kinds of honey and fruit juice samples by the prepared anion exchangeable film. After TFME, the analyte was quantified through high performance liquid chromatography-UV detection (HPLC-UV). Plackett–Burman design was employed for screening the experimental factors. The effective factors were then optimized using Box Behnken Design (BBD). Under the optimized conditions, the obtained limit of detection and limit of quantification were 0.18 and 0.61 µg L−1, respectively. Batch-to-batch reproducibility at 50 µg L−1 concentration level was 4.3% (n=3). The validation results allowed the method to be utilized in the quantification of quercetin in real samples