色谱

色谱 ›› 2012, Vol. 30 ›› Issue (10): 1031-1036.DOI: 10.3724/SP.J.1123.2012.06026

• 研究论文 • 上一篇    下一篇

超高效液相色谱/高分辨飞行时间质谱法同时检测乳制品中19种抗生素

张洁1, 严丽娟2*, 潘晨松3, 林立毅2, 张欣怡3, 申河清1*   

  1. 1. 城市环境与健康重点实验室, 中国科学院城市环境研究所, 福建 厦门 361021; 2. 厦门出入境检验检疫局, 福建 厦门 361012; 3. 美国布鲁克道尔顿公司北京代表处, 北京 100081
  • 收稿日期:2012-06-17 修回日期:2012-08-22 出版日期:2012-10-28 发布日期:2012-10-17
  • 通讯作者: 申河清,博士,研究员,主要研究方向为环境污染物的暴露科学和健康效应. Tel: (0592)6190771, E-mail: hqshen@iue.ac.cn.严丽娟,博士,高级工程师,主要研究方向为食品安全检测. Tel: (0592)3269943
  • 基金资助:

    福建省自然科学基金项目(2011J05029)和厦门市科技项目(3502Z20112017, 3502Z20102013).

Simultaneous analysis of 19 antibiotics in dairy products using ultra-performance liquid chromatography coupled with high resolution time-of-flight mass spectrometry

ZHANG Jie1, YAN Lijuan2*, PAN Chensong3, LIN Liyi2, ZHANG Xinyi3, SHEN Heqing1*   

  1. 1. Key Laboratory of Urban Environment and Health, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021, China; 2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China; 3. Bruker Daltonics Inc. Beijing Office, Beijing 100081, China
  • Received:2012-06-17 Revised:2012-08-22 Online:2012-10-28 Published:2012-10-17

PDF

498

被引次数

29

摘要： 利用超高效液相色谱/高分辨飞行时间质谱结合数据库建立了乳制品中19种抗生素的分析方法。样品依次经过乙腈和酸化乙腈处理后,冷冻离心浓缩,经超高效液相色谱分离,正离子扫描模式下,在10 min内对19种抗生素进行分离和检测,质量浓度在10～500或15～1000 μg/L范围内具有良好的线性关系,检出限为3～5 μg/L,平均回收率为68.4%～96.7%。加标样品的筛查结果表明,保留时间偏差不大于0.1 min,质量偏差小于5 mDa,同位素峰形匹配度不低于87.4%, 19种加标抗生素被全部检测出来,且大部分抗生素获得很高的鉴定评分。对购自本地超市的40余份乳制品进行了筛查分析,未检出阳性样品。该分析方法具有前处理简单、分析速度快、灵敏度高、质量精确度高的特点,可应用于乳制品中抗生素的快速筛查。

关键词: 超高效液相色谱, 飞行时间质谱, 抗生素, 牛奶, 乳制品, 筛查

Abstract: An ultra-performance liquid chromatography coupled with high resolution time-of-flight mass spectrometry method (UPLC/HRTOF-MS) has been developed for the simultaneous analysis of 19 antibiotics in dairy products. The sample was treated with acetonitrile and acidic acetonitrile to remove protein and fat, and then the supernatant was concentrated with a concentrator system. The antibiotics in the prepared sample were separated on a BEH column, and then qualitatively and quantitatively analyzed by HRTOF-MS in positive ionization mode within 10 min. A screening database containing the qualitative information of the antibiotics was built with TargetAnalysis software. Matrix matching was used in the antibiotic analysis to compensate for the matrix effects that influence analytical response. The linear range of the antibiotics was 10~500 or 15~1000 μg/L. The limits of detection (LOD) were from 3 to 5 μg/L. At the spiked levels of 20 and 100 μg/L, the average recoveries were from 68.4% to 96.7% with the relative standard deviations ranging from 2.1% to 12.5%. The screening results of a spiked milk sample showed that all the spiked antibiotics could be detected with their deviations of retention time ≤0.1 min, the deviations of mass ＜5 mDa, the degrees of isotope pattern match ≥87.4%, and most spiked antibiotics were detected with high scores. Furthermore, the developed method was applied for the analysis of antibiotics in more than 40 milk and dairy products of seven manufacturers, and the target antibiotics were not detected in all the samples. The method is rapid, sensitive and easy to operate, and is suitable for the screening of antibiotic residues in milk and dairy products.

Key words: antibiotics, dairy products, milk, screening, time-of-flight mass spectrometry (TOF MS), ultra performance liquid chromatography (UPLC)

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