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LC-MS/MS测定牛奶中7种抗生素残留
引用本文:倪炜华,蔡丹萍,陈婷,于丽芳.LC-MS/MS测定牛奶中7种抗生素残留[J].安徽农业科学,2013(18):7942-7944.
作者姓名:倪炜华  蔡丹萍  陈婷  于丽芳
作者单位:1. 嘉兴市农产品监测中心,浙江嘉兴,314050
2. 嘉兴市产品质量监督检验所,浙江嘉兴,314050
摘    要:目的]建立液相色谱质谱法检测牛奶中7种抗生素残留的试验方法。方法]将供试样品用Mcllvaine-EDTA溶液提取后,经HLB 3cc固相萃取柱净化,采用液相色谱质谱仪进行定性、定量分析,以0.2%甲酸水和0.2%甲酸乙腈为流动相,在0.20 ml/min下梯度洗脱。结果]液相色谱质谱法检测牛奶中7种抗生素残留的方法在2.0~80.0 ng/ml范围内呈良好的线性关系,平均回收率为81.0%~100.0%,相对标准偏差为2.5%~9.6%,检出限为0.01~0.10μg/kg。结论]液相色谱质谱法适用于牛奶中青霉素G、青霉素V、氨苄西林、土霉素、金霉素、四环素、强力霉素的检测。

关 键 词:液相色谱质谱法  牛奶  抗生素  固相萃取

LC-MS/MS Determination of 7 Kinds of Antibiotic Residues in Milk
Institution:NI Wei-hua( 1.Jiaxing Agriculture Products Supervision Testing Agency, Jiaxing, Zhejiang 314050;)
Abstract:Objective] To establish a method for determining 7 kinds of antibiotic residues in milk by liquid chromatography-mass spectrometry.Method] Samples were extracted by Mcllvaine-EDTA solution,after HLB 3cc solid-phase extraction (SPE),then it was analyzed by liquid chromatography-mass spectrometry with a mobile phase of 0.2% formic acid/water and 0.2% formic acid/acetonitrile at a flow rate of 0.20 ml/min by gradient elution.Result] The method showed good linearity in the range of 2.0-80.0 ng/ml,the average recovery was 81.0%-100.0%,the relative standard deviations ranged from 2.5%-9.6%,the limit of detection was from 0.01-0.10 μg/kg.Conclusion] The method was applied to determinate penicillin G,penicillin V,anpicillin,oxytetracycline,chlortetracycline,tetracycline,doxycycline in milk with satisfactory results.
Keywords:Liquid chromatography-mass spectrometry  Milk  Antibiotics  Solid phase extraction
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