表面增强拉曼光谱法快速检测猪肉中氟尼辛葡甲胺残留

氟尼辛葡甲胺（FM）是动物专用的非甾体类消炎药，是兽医临床上最常用的消炎镇痛类药物。近年来，随着其应用范围的扩大，其不良反应逐渐显现，其在兽肉中的残留引起了人们的重视。目前猪肉中FM残留的主要检测方法为色谱法、色谱质谱联用法。设备昂贵、笨重、操作复杂等缺点极大的限制了这类方法在现场快速检测中的应用，表面增强拉曼（SERS）具有指纹识别、迅速检测、便携等优势，能克服色谱技术在现场检测中带来的不便，因而近年来被广泛应用于兽药残留的快速筛查检测。因此，为实现猪肉中FM的现场快速检测，建立了猪肉中FM的SERS检测方法。用柠檬酸钠还原氯金酸钾的方法制备金溶胶，通过单因素实验确定在样品与金胶体积比为1∶3，样品pH为6，不添加促凝剂，为检测条件。用密度泛函理论计算理论光谱，结合固体拉曼光谱，对各峰进行振动模式归属。其中731 cm-1处为吡啶环、苯环摇摆，1 085和1 376 cm-1处均为苯环上C—H振动。之后通过优化萃取前处理方法与萃取剂的选取，建立了猪肉中FM的定性定量检测方法。在该方法中，FM在猪肉基质中的特征峰为731，1 085和1 376 cm-1。选取731 cm-1作为定性定量峰，该处拉曼强度与FM浓度在1～250 mg·L-1内有良好的线性关系，R2为0.99。对加标样品的实际浓度进行检测，其检测限为1 mg·L-1，回收率在89.61%～95.63%，RSD在1.80%～3.30%内。该法稳定、快速、简单，可实现FM在猪肉中的现场快速筛查检测。

Surface-Enhanced Raman Spectroscopy for Rapid Detection of Flunixin Meglumine Residues in Pork

Flunixin meglumine (FM) is the only animal-specific non-steroidal anti-inflammatory drug, and it is the most commonly used anti-inflammatory and analgesic drug in veterinary clinics. In recent years, with the expansion of its application scope, its adverse reactions gradually appeared, and the residues of Flunixin meglumine in animal meat gradually attracted people’s attention and attention. The current detection methods of FM include liquid chromatography-tandem mass spectrometry, and liquid chromatography. However, this method has disadvantages such as expensive equipment, cumbersome and complicated operation, which is highly unfavourable for rapid on-site detection. Surface-enhanced Raman spectroscopy (SERS) has the advantages of portability, rapid detection, fingerprint recognition, etc., which can overcome the chromatographic technology brought by on-site detection. Because of the inconvenience, it has been widely used in the rapid screening and detection of veterinary drug residues in recent years. Therefore, in order to realize the rapid detection of FM in pork, a rapid detection method of levamisole residues in pork by SERS was established. The gold sol was prepared by reducing potassium chloroaurate with sodium citrate. Through a single factor experiment, it was determined that when the volume ratio of sample to gold gel was 1∶3, the pH of the sample was 6, and no coagulant was added, the detection effect was the best. Combining density functional theory to calculate theoretical spectra, compare theoretical calculation spectra with solid Raman spectra, assigning vibration modes to characteristic peaks. Among them, the pyridine ring and benzene ring swing at 731, 1 085 and 1 376 cm-1 are C—H vibration on the benzene ring. After optimizing the extraction pretreatment method and the selection of extractant, a qualitative and quantitative detection method for FM in pork was established under the best detection conditions. In this method, the characteristic peaks of FM in the pork matrix are 731, 1 085 and 1 376 cm-1. Choose 731 cm-1 as the qualitative and quantitative peak, where the Raman intensity and the FM concentration have a good linear relationship within 1～250 mg·L-1, and R2 is 0.99. The actual concentration of the spiked samples was tested, the recovery rate was 89.61%～95.63%, and the RSD was 1.80%～3.30%. The method is simple, fast and stable in operation, and is beneficial to the rapid on-site detection of FM residues in pork.