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建立了水产品中氯霉素、甲砜霉素和氟甲砜霉素药物残留量同时测定的高效液相色谱-串联质谱方法。以氘代氯霉素做内标,选择乙酸乙酯提取,HLB固相萃取柱净化,洗脱液氮气吹干,采用LC-MS/MS选择反应监测(SRM)负离子模式进行定性、定量分析。结果表明:氯霉素的检出限(LOD)为0.01μg/kg,甲砜霉素和氟甲砜霉素检出限(LOD)为0.03μg/kg,检测结果的相对标准偏差为3.3%～9.7%(n=6),加标回收率达到78.6%～110.5%。该方法在水产品中氯霉素、甲砜霉素和氟甲砜霉素药物的残留测定中具有很好的应用前景。
The simultaneous determination of chloramphenicol, thiamphenicol and florfenicol in aquatic products was established by high performance liquid chromatography-tandem mass spectrometry. Chloramphenicol was used as the internal standard. Ethyl acetate extraction, HLB solid-phase extraction (SPE) column purification and nitrogen-drying of the eluent were used. Qualitative and quantitative analysis was carried out by negative ion mode of LC-MS / MS selective reaction monitoring (SRM). The results showed that the detection limit (LOD) of chloramphenicol was 0.01 μg / kg, the detection limit (LOD) of thiamphenicol and florfenicol was 0.03 μg / kg, and the relative standard deviation was 3.3% ~ 9.7% (n = 6), the recoveries of standard addition reached 78.6% ~ 110.5%. The method has good application prospect in the determination of residues of chloramphenicol, thiamphenicol and florfenicol in aquatic products.