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目的建立检测猪肉中磺胺氯哒嗪、磺胺间甲氧嘧啶、磺胺噻唑、磺胺嘧啶及磺胺吡啶等药物残留的超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)。方法样品采用乙腈提取后,浓缩提取物用正己烷脱脂净化,正离子多反应监测(multiple reaction monitoring,MRM)测定,外标法定量。结果磺胺类药物在5~200μg/L质量浓度范围内线性关系良好,相关系数R2均大于0.996。5种磺胺的检出限均为5μg/kg,在添加量为10.0~150.0μg/kg时回收率为90%~105%,相对标准偏差(relative standard deviation,RSD)≤7%。结论建立的方法精密度、准确度较高,选择性好,操作快速、简便,能对猪肉中的磺胺类残留进行定性和定量分析。
OBJECTIVE To establish a ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS) for the determination of residues of sulfadiazine, sulfamonomethoxine, sulfathiazole, sulfadiazine and sulfapyridine in pork / MS). Methods After the samples were extracted with acetonitrile, the concentrated extracts were degreased with n-hexane, and detected by multiple reaction monitoring (MRM) and external standard method. Results The sulfonamides showed a good linearity in the concentration range of 5 ~ 200μg / L, the correlation coefficient R2 was greater than 0.996. The detection limits of the five sulfonamides were 5μg / kg, and recovered at the dosage of 10.0 ~ 150.0μg / kg Rates ranged from 90% to 105% with a relative standard deviation (RSD) ≤7%. Conclusion The established method has high precision, high accuracy, good selectivity, quick and easy operation, and can qualitatively and quantitatively analyze sulfonamides residues in pork.