超高效液相色谱-串联质谱法检测饲料中氯霉素、氟苯尼考药物的方法研究

根据贵州省实际情况,试验建立浓缩饲料和配合饲料中氯霉素、氟苯尼考的超高效液相色谱串联质谱快速检测方法,作为国家饲料标准对该类物质检测的有效补充,保障贵州省动源性食品安全。称取粉碎后的饲料,加适量D5-氯霉素和D3-氟苯尼考混合工作液,经乙酸乙酯提取后,分取部分上清液,氮气吹干,水复溶,正己烷脱脂,取下层溶液过0.22μm滤膜。采用C18色谱柱分离,乙腈:水(40:60)等度洗脱。结果表明,氯霉素、氟苯尼考在0.2~10.0μg/kg范围内线性良好,相关系数均大于0.99,方法检测限和定量限都为0.2μg/kg,3个加标浓度(0.2、1.0和5.0μg/kg)的氯霉素的平均回收率在80.2%~116.0%之间,氟苯尼考的平均回收率在82.4%~113.5%,相对标准偏差小于15%。试验结果完全符合饲料相关国家标准检测需求,适用于浓缩饲料和配合饲料中氯霉素、氟苯尼考定性定量检测。

Determination of chloramphenicol and florfenicol in feed by UPLC MS/MS

According to the actual situation of Guizhou province, the experiment established a rapid detection method of chloramphenicol and florfenicol in concentrated feed and compound feed by UPLC-MS/MS, as an effective supplement to the national feed standard for the detection of such substances, to ensure the safety of Guizhou province’s dynamic food. Weighed the crushed feed, added appropriate amount of chloramphenicol D5 and florfenicol D3 mixed working solution, extracted it with ethyl acetate, took part of the supernatant, dried it with nitrogen, dissolved it in water again, degreased it with n-hexane and took the lower solution and filter took it through 0.22 μm filter membrane. C18 column was used for separation, acetonitrile: water(40:60) isocratic elution. The results showed that the linearity of chloramphenicol and florfenicol was good in the range of 0.2~10.0 μg/kg, the correlation coefficient was greater than 0.99, the detection limit and quantitative limit were both 0.2 μg/kg, the average recovery of chloramphenicol in three standard concentrations(0.2, 1.0 and 5.0 μg/kg) was 80.2%~116.0%, the average recovery of florfenicol was 82.4%~113.5%, and the relative standard deviation was less than 15%. The results of the test completely meet the requirements of the national standards for the detection of feed, and it is suitable for the qualitative and quantitative detection of chloramphenicol and florfenicol in concentrated feed and compound feed.