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

发布时间：2018-08-14 12:21

【摘要】：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N_2吹干,残渣用10%乙腈水溶液溶解,正己烷除脂,采用BEH C_18(2.1 mm×50 mm,1.7μm)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0.51~20.8μg/kg浓度范围呈良好的线性关系,R~2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0.158~0.173μg/kg,定量限为0.475~0.52μg/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。
[Abstract]:Objective: to establish a method for the simultaneous determination of chloramphenicol, sulfadiazine, sulfathiazole, trimethoprim and sulfadiazine residues in pork by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods: after adding ethyl acetate, pork was homogenized, the organic layer N2 was blown dry, the residue was dissolved in 10% acetonitrile solution, n-hexane was degreased, BEH C18 (2.1 mm 脳 50 mm ~ 1.7 渭 m) column was used to separate the residue, and acetonitrile and water were used as mobile phase for gradient elution. Electrospray ion source (ESI), was used to monitor (MRM). Results: under this experimental condition, The linear range of chloramphenicol and sulfamethylamine was 9.6v 384and 0.51g 20.8 渭 g/kg, the detection limit of chloramphenicol was 3.2 ng / kg, the limit of quantification was 9.6 ng / kg, the detection limit of 5 sulfonamides was 0.1580.173 渭 g / kg, the quantitative limit was 0.475U 0.52 渭 g / kg, the detection limit of chloramphenicol was 3.2ng / kg, the quantitative limit was 9.1580.173 渭 g / kg, and the quantitative limit was 0.475g / kg. The average recovery range was 70.84 and 103.99, and the relative standard deviation was 1.988.01. Conclusion: this method is simple, rapid, sensitive and accurate.
【作者单位】：贵州医科大学药学院;贵州医科大学贵州省药物制剂重点实验室;贵州医科大学民族药与中药开发应用教育部工程研究中心;
【基金】：贵州省高等学校创新能力提升计划(黔教合协同创新字[2013]04) 贵州省优青项目(黔科合人字[2015]11号) 现代药物研究开发协同创新中心(黔教合协同创新字[2013]04)
【分类号】：O657.63;TS251.51

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