超高效液相色谱-串联三重四极杆质谱法测定猪肉及猪肝中56种抗生素残留量  

Determination of 56 kinds of antibiotics residues in pork and swine liver using ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry

作　　者：刘晓晔 张柏铭 王宏宇 王晓茵[2] 孙晓亮[2] 李木子 方汉卿 曹旭敏[2] 万思敬 秦立得 LIU Xiao-Ye;ZHANG Bai-Ming;WANG Hong-Yu;WANG Xiao-Yin;SUN Xiao-Liang;LI Mu-Zi;FANG Han-Qing;CAO Xu-Min;WAN Si-Jing;QIN Li-De(School of Animal Medicine,Qingdao Agricultural University,Qingdao 266109,China;China Animal Health and Epidemiology Center,Qingdao 266032,China;Hebei Provincial Animal Epidemic Control Center,Shijiazhuang 050035,China;Qingdao Agricultural Products Quality and Safety Center,Qingdao 266100,China)

机构地区：[1]青岛农业大学动物医学院,青岛266109 [2]中国动物卫生与流行病学中心,青岛266032 [3]河北省动物疫病预防控制中心,石家庄050035 [4]青岛市农产品质量安全中心,青岛266100

出　　处：《食品安全质量检测学报》2024年第23期274-286,共13页Journal of Food Safety and Quality

基　　金：中国动物卫生与流行病学中心创新基金项目(DW2022005)。

摘　　要：目的建立一种检测猪肉和猪肝中喹诺酮类、磺胺类、大环内酯类、四环素类、林可酰胺类、截短侧耳类共6类56种抗生素残留的固相萃取(solid phase extraction,SPE)-超高效液相色谱-串联三重四极杆质谱(ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry,UPLC-MS/MS)法。方法使用2种不同的提取液[2 mL乙二胺四乙酸(ethylenediaminetetraacetic acid,EDTA)-McIlvaine缓冲液、1.5 mL甲醇和4.5 mL乙腈与8 mL乙腈]先后提取样品中目标药物,经正己烷去脂,使用HLB固相萃取柱净化,3 mL洗脱液(甲醇:乙酸乙酯=7:3,V:V)洗脱,采用UPLC-MS/MS检测。结果56种抗生素在2~100μg/kg范围内线性关系良好,相关系数均大于0.990。该方法检出限为0.2~2.0μg/kg,定量限为0.6~4.5μg/kg。猪肉样品中大部分抗生素(83.93%)回收率为60.04%~106.59%,猪肝样品中大部分抗生素(83.93%)回收率为50.04%~124.41%。采用本方法对市售20份猪肉样品和13份猪肝样品检验,只有1份猪肝样品中检出恩诺沙星残留,且残留浓度低于国家标准。结论此方法灵敏度较高、重现性好,可用于猪肉和猪肝中目标抗生素残留含量准确检测,满足日常动物源性食品安全监测和风险监测的需求,为保障动物产品安全提供技术支撑。Objective To establish a method that validates for the simultaneous detection of 56 kinds of antibiotic residues belong to 6 classes,namely,quinolones,sulfonamides,macrolides,tetracyclines,lincosamides,and pleuromutilins,in pork and swine liver samples using solid phase extraction(SPE)and ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry(UPLC-MS/MS).Methods The 2 different extracts[2 mL ethylenediaminetetraacetic acid(EDTA)-McIlvaine buffer,1.5 mL methanol,4.5 mL acetonitrile,and 8 mL acetonitrile]were used to extract target antibiotics from pork and swine liver samples.These extractions were defatted by n-hexane,cleaned up with HLB solid-phase extraction columns,eluted with 3 mL elution(methanol:ethyl acetate=7:3,V:V)and analyzed by UPLC-MS/MS.Results The 56 kinds of antibiotics exhibited strong linear relationships within the range of 2-100μg/kg,with all linear correlation coefficients exceeding 0.990.The limits of detection this method ranged from 0.2μg/kg to 2.0μg/kg,and the limits of quantification varied between 0.6μg/kg and 4.5μg/kg.The recovery rate of 83.93%target antibiotic in pork was 60.04%-106.59%,whereas the rate of 83.93%target analyts in swine liver falled within a range of 50.04%to 124.41%.Enrofloxacin residue was detected in only one swine liver sample out of 20 pork samples and 13 swine liver samples using this method,with the residual concentration being below the national standard.Conclusion This method exhibits high sensitivity and reproducibility,enabling the simultaneous determination of various antibiotics in pork and swine liver products.It meets the requirements for daily food safety monitoring and potential risks detection of target analytes in animal products,offering technical support to ensure the safety of these products.

关 键 词：抗生素残留 猪肉 猪肝 固相萃取 超高效液相色谱-串联三重四极杆质谱法 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]