摘要
目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定牛奶中环丙沙星、恩诺沙星、氧氟沙星(3种氟喹诺酮类药物)、氯霉素、甲砜霉素、氟苯尼考(3种酰胺醇类)、氮氨菲啶(1种抗锥虫药)7种兽药残留的方法。方法牛奶样品经乙腈/0.5 mmol/L甲酸铵甲醇溶液(1:1,V:V)提取,正己烷净化,氮气吹干,运用UPLC-MS/MS对牛奶样本中7种兽药进行同时测定,基质匹配外标法定量。结果牛奶基质中7种兽药的线性范围为1.0~200.0μg/L,线性关系良好(r^(2)均大于0.993),检出限为0.08~0.44μg/kg,定量限为0.28~1.46μg/kg。牛奶基质对7种兽药均产生增强的基质效应。7种兽药在低、中、高3个浓度水平的加标回收率分别为47.44%~117.89%、82.34%~112.84%、73.15%~117.69%,相对标准偏差为1.46%~8.26%。采用该方法对9份市售牛奶样本进行分析,均未检出7种兽药残留。结论该方法灵敏度高,操作简便,能够满足牛奶中7种兽药的快速准确检测。
Objective To establish a method for the simultaneous determination of 7 kinds of veterinary drug residues,including ciprofloxacin,enrofloxacin,ofloxacin(3 kinds of fluoroquinolones),chloramphenicol,thiamphenicol,flufenicol(3 kinds of amphenicols)and isometamidium(1 kind of antitrypanosomal drugs)in milk by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Milk samples were extracted by the mixture of acetonitrile and 0.5 mmol/L ammonium formate in methanol(1:1,V:V),purified by n-hexane,dried by nitrogen.The 7 kinds of veterinary drug residues in milk samples were detected by UPLC-MS/MS and quantified by matrix matching external standard method.Results The linear range of 7 kinds of veterinary drugs in milk was 1.0–200.0μg/L with good linearity(r^(2) were all greater than 0.993).The limits of detection were 0.08–0.44μg/kg,and the limits of quantitation were 0.28–1.46μg/kg.Milk matrix had an enhanced matrix effect on all 7 kinds of veterinary drugs.The recoveries of 7 kinds of veterinary drugs at low,medium and high concentrations were 47.44%–117.89%,82.34%–112.84%,73.15%–117.69%,respectively.The relative standard deviations were 1.46%–8.26%.This method was used to analyze 9 samples of commercially available milk,and no residues of 7 kinds of veterinary drugs were detected in any of them.Conclusion This method is highly sensitive and easy to operate,and can meet the rapid and accurate detection requirements of seven kinds of veterinary drugs in milk.
作者
李聪
郑懿
林彬
刘雪芹
王红亮
王赤华
LI Cong;ZHENG Yi;LIN Bin;LIU Xue-Qin;WANG Hong-Liang;WANG Chi-Hua(Huanggang Municipal Center for Disease Control and Prevention,Key Laboratory of Food Safety Risk Monitoring for Health Commission of Hubei Province,Huanggang 438000,China)
出处
《食品安全质量检测学报》
2026年第4期113-120,共8页
Journal of Food Safety and Quality
基金
湖北省自然科学基金项目(2025AFB453)
黄冈市疾控人才发展专项(42110022237T000000187)。
关键词
牛奶
兽药残留
超高效液相色谱-串联质谱法
milk
veterinary drug residues
ultra performance liquid chromatography-tandem mass spectrometry
