Abstract: Fluoroquinolones and amphenicols are widely used as broad-spectrum and high-efficiency antibiotics in livestock and poultry production, but excessive drug residues frequently occur. Liquid chromatographic and liquid chromatographic mass spectrometry are the primary methods to detect the fluoroquinolones and amphenicols. According to the current domestic standard, these two veterinary drug residues can only be detected in milk simultaneously, and there are few reports in other matrices. Therefore, it is urgent to establish and optimize the simultaneous detection methods of fluoroquinolones and amphenicols in different matrices. This paper summarizes four standard pretreatment techniques such as liquid-liquid extraction, solid-phase extraction, QuEChERS method and accelerated solvent extraction, and discusses the application of hotspot nanomaterial adsorbent in detail. From the perspective of chromatography and chromatography mass spectrometry, the effects of different matrix conditions, instrument conditions and liquid phase conditions on the performance parameters of the method are summarized and discussed to provide a reference for the detection and supervision of veterinary drug residues in animal-derived foods.