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<b>Objective:</b> This study aimed to establish a method for the Preparation of matrix reference material for carbaryl residues in Chinese yam flour. <b>Methods:</b> Yam powder containing menafyl was prepared by homogenized, freeze-dried, ground, sifted, mixed and packaged. A liquid chromatography-series mass spectrometer was used for detection, and the isotope internal standard curve method was used for quantification. Through the process of equalization stability evaluation, cooperative setting and uncertainty evaluation, the matrix reference material of the expected yam powder was obtained. <b>Results:</b> The property value and expanded uncertainty of carbaryl was (1.04±0.10) mg/kg (<i>k</i>=2). <b>Conclusion:</b> It could be used for food laboratory method verification, quality control and other activities.