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目的建立超高效液相色谱-串联质谱法测定河蟹中氯霉素类药物残留的方法。方法采用1%高氯酸水溶液除蛋白质,正己烷除脂肪,乙酸乙酯提取,Oasis HLB固相萃取小柱净化后,超高效液相色谱-串联质谱测定。色谱柱:BEH C18(2.1×100 mm,1.7μm);柱温:35℃;样品室温度:4℃;流动相:A相为甲醇,B相为水,梯度洗脱;流速:0.35 ml/min;进样体积:7μl;多反应监测(MRM)模式检测。结果氯霉素、氟苯尼考、甲砜霉素方法检出限分别为0.01μg/kg、0.01μg/kg、0.02μg/kg,方法回收率在85%~110%之间,相对标准偏差RSD均小于10%。结论本方法适用于河蟹中氯霉素、甲砜霉素、氟苯尼考的检测。
Objective To establish a method for the determination of chloramphenicol residues in crabs by ultra performance liquid chromatography-tandem mass spectrometry. Methods 1% perchloric acid aqueous solution was used for protein removal, n-hexane removal of fat, extraction with ethyl acetate and purification with Oasis HLB solid phase extraction cartridges, followed by ultra performance liquid chromatography-tandem mass spectrometry. Column: BEH C18 (2.1 × 100 mm, 1.7 μm); column temperature: 35 ° C; sample compartment temperature: 4 ° C .; mobile phase: methanol in phase A and water in gradient phase B; min; injection volume: 7μl; multiple reaction monitoring (MRM) mode detection. Results The detection limits of chloramphenicol, florfenicol and thiamphenicol were 0.01 μg / kg, 0.01 μg / kg and 0.02 μg / kg, respectively. The recoveries were between 85% and 110%. The relative standard deviations RSD less than 10%. Conclusion This method is suitable for the detection of chloramphenicol, thiamphenicol and florfenicol in crabs.