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采用超高效液相色谱-串联质谱仪(UPLC-MS/MS)同时快速测定鱼用配合饲料中的氯霉素、甲砜霉素和氟苯尼考3种药物。样品由乙酸乙酯2次提取,经旋蒸浓缩、流动相溶解、正己烷净化后,采用超高效液相色谱C18柱,以5 mmol/L乙酸铵溶液-甲醇作流动相梯度洗脱分离,电喷雾负离子多反应监测模式(MRM)检测,内标法定量。氯霉素和氟苯尼考的定量限均为0.30μg/kg,线性范围均为0.20~50.0μg/L;甲砜霉素的定量限为0.5μg/kg,线性范围为0.5~50.0μg/L。氯霉素在0.5、1.0、4.0μg/kg和甲砜霉素、氟苯尼考在2.0、10.0、50.0μg/kg的添加水平上的加标回收率为79.8%~102.5%,所有测定结果的日内和日间相对标准偏差(RSD)均小于15%。该方法简便快捷,准确度和精密度高,能够满足鱼用配合饲料中氯霉素类药物同时检测的要求。
Simultaneous rapid determination of three drugs chloramphenicol, thiamphenicol and florfenicol in fish feed with UPLC-MS / MS. The sample was extracted twice with ethyl acetate, concentrated by rotary evaporation, dissolved in the mobile phase, and purified with n-hexane. The residue was purified by ultra performance liquid chromatography C18 column with 5 mmol / L ammonium acetate-methanol as mobile phase. Electrospray negative ion multiple reaction monitoring mode (MRM) detection, internal standard method. The limits of quantification of chloramphenicol and florfenicol were both 0.30μg / kg and the linear range was 0.20-50.0μg / L respectively. The limit of quantification of thiamphenicol was 0.5μg / kg and the linear range was 0.5-50.0μg / L. The spiked recoveries of chloramphenicol at the addition levels of 0.5, 1.0, 4.0 μg / kg and thiamphenicol and florfenicol at the concentrations of 2.0, 10.0 and 50.0 μg / kg ranged from 79.8% to 102.5% Day and day relative standard deviations (RSDs) were less than 15%. The method is simple, rapid, accurate and precise, and can meet the requirement of simultaneous detection of chloramphenicol in fish feed.