高效液相色谱-串联质谱法测定猪肉中氯霉素和五种磺胺类药物的残留量

摘要

Objective:A method of determination of chloramphenicol,sulfamerazine,sulfadimidine,sulfathiazole,trimethoprim,and sulfadiazine in pork by ultra-high liquid chromatography-tandem mass spectromrtry (UPLC-MS/MS)was developed.Method:Samples were extracted with ethyl acetate precipitated protein at the same time and dried under nitrogen.The residue was dissolved with 10％ acetonitrile solution and defatted by cyclohexane.Samples were detected by UPLC-MS/MS and isolated with UPLC BEH C18.The liquid phase was acetonitrile and water.The electrospray ionization (ESI)mass spectrometry had run in multiple reaction monitoring mode (MRM).Result:At these experimental conditions,chloramphenicol had good liner relatively(R2 ＞ 0.99) between 9.6 ～ 384 ng/kg.And sulfamerazine,sulfadimidine,sulfathiazole,trimethoprim and sulfadiazine had good liner relatively(R2 ＞ 0.99) between 0.51 ～20.8 μg/kg.Limits of detection were 3.2 ng/kg for chloramphenicol,0.158～ 0.173 μg/kg for 5 kinds of sulfonamides (sulfamerazine,sulfadimidine,sulfathiazole,trimethoprim,sulfadiazine).Limits of quantitation were 9.6 ng/kg for chloramphenicol,0.475～0.52 μg/kg for 5 kinds of sulfonamides(sulfamerazine,sulfadimidine,sulfathiazole,trimethoprim and sulfadiazine).Average recoveries were 70.84％～ 103.99％ with relative standard deviations of 1.98％～8.01％.Conclusion:This method could detect the chloramphenicol,sulfamerazine,sulfadimidine,sulfathiazole,trimethoprim,and sulfadiazine residue in pork with a better precision,higher accuracy and better specificity.%目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时快速测定猪肉中氯霉素、磺胺甲嘧啶、磺胺二甲嘧啶、磺胺噻唑、甲氧苄啶和磺胺嘧啶残留量的分析方法.方法:猪肉加入乙酸乙酯后匀浆,转移有机层N2吹干,残渣用10％乙腈水溶液溶解,正己烷除脂,采用BEH C18(2.1 mm×50 mm,1.7 μm)色谱柱分离,以乙腈和水为流动相进行梯度洗脱,采用电喷雾离子源(ESI),以多反应监测(MRM)方式检测.结果:在该实验条件下,氯霉素和5种磺胺类药物分别在9.6～384 ng/kg和0.51～20.8 μg/kg浓度范围呈良好的线性关系,R2均大于0.99;氯霉素检出限为3.2 ng,/kg,定量限为9.6 ng/kg,5种磺胺类药物检出限为0.158～0.173 μg/kg,定量限为0.475～0.52 μg/kg;方法的平均回收率范围为70.84％ ～ 103.99％,相对标准偏差为1.98％～8.01％.结论:此方法具有简便快捷、灵敏度高、定量准确等特点.