高效液相色谱-串联质谱法同时检测虾肉和猪肉中氯霉素、甲砜霉素、氟苯尼考和其代谢产物氟苯尼考胺残留

Simultaneous Determination of Residues of Chloramphenicol, Thiamphnicol, Florfenicol and Florfenicol Amine in Shrimp Muscle and Pork by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法同时检测虾肉和猪肉中氯霉素、甲砜霉素、氟苯尼考和其代谢产物氟苯尼考胺残留。以2％碱性乙酸乙酯提取，省去固相萃取（SPE）和液-液萃取（LPE）脱脂，浓缩后采用甲醇和5mmol／L乙酸铵以0．25mL／min流速梯度洗脱，LC—MS／MS电喷雾电源（ESI），负离子，选择反应监测（SRM）模式检测。试验结果表明：4种药物在0．1～20μg，L的范围内线性良好，相关系数尺。在0．9997～0．9998之间。在添加量为1．00。5．00μg／kg时，平均回收率在78．17％～99．86％之间，RSD在2．18％。9．27％之间。氯霉素、甲砜霉素、氟苯尼考和氟苯尼考胺的检出限分别为0．001，0．020，0．002，0．003μg／kg。

A high performance liquid chromatography-tandem mass spectrometry method was developed for simultane-ous determination of Chloramphenicol （CAP）, Thiamphnicol （TAP）, Florfenicol （FF） and Florfenicol amine （FFA） in shrimp muscle and pork. The samples were extracted with 2% basic ethyl acetate. Concentrated extracts were no liquid-liquid partition and solid phase extraction （SPE） procedure. The gradient elution solvent of methanol and 5 mmol/L am- monium acetate at a flow rate of 0.25 mL/min. Identification was achieved by electro spray ionization （ESI） in negative mode using selected reaction monitoring. The calibration curves were good linear between the peak areas and the con-centrations of 0.1-20 μg/L, and the correlation coefficients （R2） were between 0.9997-0.9998. The average recoveries and relative standard deviations （RSDs） for the analysis of all samples fortified over the range of 1.00-5.00 μg/kg were in the range of 78.17%-99.86% and 2.18%-9.27%, respectively. The limit of detection of chloramphenicol, thiamphenicol, flor-fenicol and florfenicol amine were 0.001, 0.020, 0.002 μg/kg and 0.003 μg/kg.