Composite multilayer firms composed of polyoxometalate α/β-K6P2W18O62·xH2O and polyelectrolyte PAA were attached to the bare glassy carbon (GC) electrode by Layer-by-Layer self-assembly method. Cyclic voltammetry technique was used to study the electrochemical properties of the [PSS/P2W18] modified electrode on sodium metabisulphite. The results showed that the electrode had a significantly electrocatalytic activity on the oxidation of samples. There is a liner relationship between the concentrations of the sodium metabisulphite and the response current, the calibration equations and regression coefficients were:I (mA)=0.070 6c-0.003 5,r=0.999 3 for sodium metabisulphite in the range of 0.04 mmol/L-0.72 mmol/L. The electrode used to analysis of the biscuit sample can get a good result, which recovery is 90.13%-111.58%. The method shows prominent advantages, such as rapid, simpleness and preciseness, which should be promising for detection of sodium metabisulphite in the biscuit, providing a theoretical basis for the novel rapid detection of sodium metabisulphite.%采用层接层法（Layer-by-layer）将聚电解质PSS与多金属氧酸盐α/β-K6P2W18O62·xH2O交替沉积到空白玻碳电极上制得多层膜电化学传感器，通过循环伏安法研究该电极对焦亚硫酸钠的电催化作用，结果表明，该电极对焦亚硫酸钠具有很明显的电催化作用。焦亚硫酸钠在0.04 mmol/L~0.72 mmol/L的浓度范围内与催化电流呈现良好的线性关系，I （mA）=0.0706c-0.0035，r=0.9993，在此范围内可对饼干中焦亚硫酸钠的含量进行测定.将该电极应用于饼干样品的分析，回收率为90.13%~111.58%，取得了较好的结果。该电极制备简单、响应快、灵敏度高、检测限低，为焦亚硫酸钠的新型快速检测提供了重要的理论依据。
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