高效液相色谱-高分辨质谱法快速筛查动物源性药食同源产品中32种抗生素兽药残留

Rapid screening of 32 kinds of veterinary drug residues in animal-derived medicine and food homologous products by high performance liquid chromatography-high resolution mass spectrometry

目的建立高效液相色谱-高分辨质谱法(high performance liquid chromatography-high resolution mass spectrometry,HPLC-HRMS)对鹿茸、鹿胎膏和蜂蜜中β-内酰胺类、林可酰胺类、大环内脂类、硝基咪唑类、喹诺酮类、磺胺类、氯霉素类共32种抗生素残留的快速前处理和筛查方法。方法动物源性产品采用乙腈超声提取,上清液经PRi ME HLB固相萃取柱(无需活化和平衡)净化,氮吹至0.5 mL以内,用10%甲醇溶解定容后,经C18色谱柱立分离,在电喷雾正离子模式下,根据32种抗生素药物的分子离子峰、特征离子信息建立HPLC-HRMS数据库,采用Trace Finder 2.5软件系统进行定性筛查和分析。结果本方法能够在缺乏标准品的前提下,迅速且准确地识别动物源性药食同源特色产品(鹿茸、鹿胎膏和蜂蜜)中的32种抗生素残留,检出限为0.01 mg/kg,准确率为100%。结论本方法简单、快速、准确,适用于大批量动物源性药食同源产品中抗生素类兽药残留的快速筛查,可为动物源性药食同源特色产品抗生素类兽药的监管提供可靠的技术支持。

Objective To establish a rapid pre-treatment and instrument screening method for 32 kinds of antibiotic residues in animal-derived medicine and food homologous products(pilose antler,semifluid extract of deer foetus and honey)based on the high performance liquid chromatography-high resolution mass spectrometry(HPLC-HRMS).Methods The samples were extracted by acetonitrile,purified by PRiME HLB solid phase extraction column,and qualitatively screened by HPLC-HRMS database(compound name,molecular formula,molecular weight,retention time,fragment ions,etc.).Results This method could quickly and accurately screen 32 kinds of antibiotic residues in animal-derived medicine and food homologous characteristic products(deer antler,deer fetal paste and honey)without standard products,with the limit of detection of 0.01 mg/kg.Conclusion This method is simple,rapid,accurate and suitable for the screening of veterinary drug residues of antibiotics in large quantities of samples,which can provide reliable technical support for the supervision of antibiotics veterinary drug residues in animal-derived medicine and food homologous products.