基质固相分散-高压液相色谱-高分辨质谱法测定猪肉中22种磺胺类药物的残留

Determination of twenty-two sulfonamide residues in pork by matrix solid phase dispersion-high pressure liquid chromatography-high resolution mass spectrometry spectrometry

中文关键词:  高分辨质谱  基质固相分散  猪肉  磺胺

英文关键词:high resolution mass spectrometry  matrix solid phase dispersion  pork  sulfonamides

中文摘要:

      目的 建立基质固相分散-高压液相色谱-高分辨质谱测定猪肉中22种磺胺类药物残留量的测定方法, 包括磺胺苯酰、磺胺醋酰、磺胺氯哒嗪、磺胺嘧啶、磺胺间二甲氧嘧啶、磺胺二甲嘧啶、磺胺甲基嘧啶、磺胺多辛、磺胺间甲氧嘧啶、磺胺甲氧哒嗪、磺胺对甲氧嘧啶、磺胺甲噁唑、磺胺甲噻二唑、磺胺二甲噁唑、磺胺苯吡唑、磺胺吡啶、磺胺喹噁啉、磺胺噻唑、磺胺异噁唑、磺胺胍、甲氧苄啶、磺胺索嘧啶。方法 猪肉样品与弗罗里硅土混合, 研磨均匀, 装入空的固相萃取管中, 用15 mL 1%乙酸二氯甲烷: 乙酸乙酯(1∶3, v/v)洗脱, 洗脱液用氮气吹干, 残渣用1 mL乙腈: 10 mmol/L乙酸铵溶液(15∶85, v/v)溶解。加入1 mL正己烷混合离心, 取下层溶液, 经0.22 μm滤膜过滤后用Agilent Poroshell 120 EC-C18(2.1 mm×150 mm, 2.7 μm)色谱柱分离, 高分辨质谱测定。结果 22种磺胺类药物在 10~100 μg/kg范围内线性关系良好, 相关系数r>0.99, 除磺胺甲噻二唑、甲氧苄啶和磺胺脒/磺胺胍加标回收率小于40%外, 其余均大于60%, 定量限为 5~10 μg/kg。结论 本方法具有前处理快速、高效、有机试剂用量少、成本小等优点, 适用于猪肉中磺胺类药物残留量的测定。

英文摘要:

      Objective To establish a method for determination of 22 sulfonamides in pork, including sulfabenzamide, sulfacetamide, sulfachloropyridazine, sulfadiazine, sulfadimethoxine, sulfamethazine, sulfamera-zinesulfadoxine, sulfamonomethoxine, sulfamethoxypyridazine, sulfamethoxydiazine, sulfamethoxazole, sulfamethizole, sulfamoxole, sulfaphenazole, sulfapyridine, sulfaquinoxaline, sulfathiazole, sulfisoxazole, sulfaguanidine, trimethoprim and sulfisomidine, with matrix solid phase dispersion and high pressure liquid chromatography-high resolution mass spectrometry. Methods Pork samples were mixed and grinded with solid-phase sorbent (Florisil), then put in a glass mortar. The mixture was packed as a solid phase extraction cartridge and eluted with 15 mL 1% acetic acid dichloromethane:ethyl acetate(1:3, v/v). The eluted materials were collected and evaporated to dry by nitrogen gas. The residues were dissolved in 1 mL acetonitrile: 10 mmol/L ammonium acetate (15:85, v/v) and 1mL n-hexane. After centrifugation, the lower solution was gone through a 0.22 μm filter membrane and then separated by Agilent Poroshell 120 EC-C18 column (2.1 mm×150 mm, 2.7 μm), after that it was determined by high resolution mass spectrometry. Results The linear range of 22 sulfonamides were 10~100 μg/kg, r>0.99. The recoveries of sulfamethizole, trimethoprim and sulfaguanidine were below 40%, the others were above 60%. The limits of quantitation were 5~10 μg/kg. Conclusion The advantages of this method are fast, efficient, less organic reagent and low cost. It is suitable for the determination of sulfonamides residues in pork.