1：Experimental Design and Method Selection:

Used multivariate curve resolution-alternating least squares (MCR-ALS) with electrochemical techniques for simultaneous determination. Response surface methodology (RSM) with central composite rotatable design (CCRD) was employed for optimization.

2：Sample Selection and Data Sources:

Real samples of chili and ketchup sauces were purchased from a local market and treated with ethanol extraction. Synthetic mixtures of Sudan II and III were prepared in ethanol.

3：List of Experimental Equipment and Materials:

Instruments include Potentiostat-Galvanostat Autolab PGSTAT30, Potentiostat Sama 500, X-ray diffractometer SIEMENS D5000, scanning electron microscope MIRA3TESCAN-XMU. Materials include Sudan II, Sudan III, zinc nitrate, sodium carbonate, graphite powder, paraffin oil, ethanol, phosphate buffers.

4：Experimental Procedures and Operational Workflow:

Synthesis of ZnONPs via precipitation method, fabrication of carbon paste electrode (CPE) and ZnONPs-modified CPE, electrochemical measurements using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and differential pulse voltammetry (DPV) with varying pulse heights to generate second-order data. Optimization of variables (pH, ZnONPs amount, scan rate, step potential) using CCRD and RSM. Application of MCR-ALS to resolve overlapping voltammetric peaks.

5：Data Analysis Methods:

MCR-ALS with non-negativity and unimodality constraints for peak decomposition, calibration curves based on peak areas, statistical analysis using MINITAB software for optimization.