气相色谱串联质谱法检测鱼肉中酰胺醇类兽药残留
GC-MS Spectrometry for Detection of Amide Alcohol and Veterinary Drug Residues in Fish Meat

建立了同时检测鱼肉中氯霉素(CAP)、氟苯尼考(FF)、氟苯尼考胺(FAH)及甲砜霉素(TAP)兽药残留的气相色谱串联质谱法。通过优化气相色谱条件实现良好的分离条件，对氯霉素、氟苯尼考、氟苯尼考胺及甲砜霉素的三甲基硅衍生物的一级离子碎片进行碰撞优化出对应的离子对作为定性定量的依据。采取2%氨化乙酸乙酯提取，MCX固相小柱净化，加入100 uL BSTFA + TMCS (99 + 1)硅烷化试剂，在65℃反应30 min。用EI源的GC-MS/MS法，选择离子(MRM)进行定性定量，相关系数 > 0.99，线性范围1~1000 ug/L，草鱼肉糜试样中加标回收率在86.2%~94.4%之间，相对标准偏差小于5%，检出限为0.1 ug/kg。
A gas chromatography-mass spectrometry was established for the simultaneous detection of chloramphenicol (CAP), florfenicol (FF), florfenicol (FAH), and thiamethoxam (TAP) veterinary drug residues in fish meat. By optimizing the gas chromatography conditions to achieve good separation conditions, collision optimization was performed on the primary ion fragments of chloramphenicol, florfenicol, florfenicoline, and trimethylsilyl derivatives of methicillin to obtain corresponding ion pairs as the basis for qualitative and quantitative analysis. Using 2% ammoniated ethyl acetate for extraction and MCX solid-phase column purification, 100 μL of BSTFA + TMCS (99 + 1) silane reagent was added and reacted at 65°C for 30 minutes. The qualitative and quantitative analysis was performed by GC-MS/MS with an EI source, using multiple reaction monitoring (MRM) for ion selection. The correlation coefficient was greater than 0.99, with a linear range of 1 to 1000 μg/L. The recovery rate of spiked grass carp minced meat samples was between 86.2% and 94.4%, with a relative standard deviation of less than 5%. The detection limit was 0.1 μg/kg.