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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 被引量:21

Simultaneous Determination of Residues of Chloramphenicol, Thiamphnicol, Florfenicol and Florfenicol Amine in Shrimp Muscle and Pork by High Performance Liquid Chromatography-Tandem Mass Spectrometry
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摘要 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.
出处 《中国食品学报》 EI CAS CSCD 北大核心 2014年第1期232-238,共7页 Journal of Chinese Institute Of Food Science and Technology
基金 湛江市财政资金科技专项(2011D02)
关键词 高效液相色谱 串联质谱 氯霉素 甲砜霉素 氟苯尼考 氟苯尼考胺 虾肉 猪肉 残留 high performance liquid chromatography-tandem mass spectrometry chloramphenicol thiamphnicol florfenicol florfenicol amine shrimp muscle pork residue
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