摘要
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 An ultra performance liquid chromatography–tandem mass spectrometry（UPLC-MS/MS） method was developed for determination of chloramphenicol（CAP）,thiamphnicol（TAP）,florfenicol（FF） residues in river crab.Methods The samples was treated with 1% perchloric acid to remove protein and n-hexane to remove fat,then extracted with ethyl acetate,and determined by UPLC-MS/MS under MRM mode after purification on Oasis HLB SPE column.The chromatographic condition were BEH C18（2.1 ×100 mm,1.7 μm）,column temperature at 35 ℃,room temperature for placing sample at 4 ℃,methanol and water as mobile phase for gradient elution,flow rate at 0.35 ml/min and injection volume of 7 μl.Results The detection limits of CAP and FF and TAP were 0.01 μg/kg,0.01 μg/kg,0.02 μg/kg.The recoveries of method was 85%~110%.The RSD of method was less than 10%.Conclusion The method was suitable for determination of chloramphenicol,thiamphnicol,florfenicol residues in river crab.
出处
《中国卫生检验杂志》
北大核心
2013年第13期2726-2729,共4页
Chinese Journal of Health Laboratory Technology
