色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 524-528.DOI: 10.3724/SP.J.1123.2014.01008

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定动物源性食品中的磺胺增效剂

高洋洋1, 张朝晖1, 刘鑫1, 卢晓宇1, 严华1, 何悦1, 杨大进2, 云环1   

  1. 1. 北京出入境检验检疫局技术中心, 北京 100026;
    2. 国家食品安全风险评估中心, 北京 100021
  • 收稿日期:2014-01-06 修回日期:2014-03-18 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 云环
  • 基金资助:

    科技部质检公益行业科研专项（201210029）；国家高技术研究发展计划（“863”计划）项目（2012AA101603）.

Determination of sulfonamide potentiators in animal origin foods by ultra performance liquid chromatography-tandem mass spectrometry

GAO Yangyang1, ZHANG Zhaohui1, LIU Xin1, LU Xiaoyu1, YAN Hua1, HE Yue1, YANG Dajin2, YUN Huan1   

  1. 1. Technology Center of Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China;
    2. China National Center for Food Safety Risk Assessment, Beijing 100021, China
  • Received:2014-01-06 Revised:2014-03-18 Online:2014-05-08 Published:2014-04-26

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摘要：

建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）测定多种基质（鸡肉、鱼肉、鸡肝、鸡蛋和牛奶）中三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶的分析方法。样品用甲酸-乙腈（1：9，v/v）溶液提取，正己烷除脂净化，Acquity UPLC BEH C18柱（50 mm×2.1 mm，1.7 μm）分离，以甲醇和5 mmol/L醋酸铵（含0.1%（v/v）甲酸）作为流动相进行梯度洗脱，电喷雾正离子（ESI+）模式电离，多反应监测（MRM）模式检测。考察了3种提取溶液的提取效率，优化了净化条件和浓缩条件，并对流动相、柱温和固相萃取柱进行了优化。结果表明：三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶在1.25~30.0 μg/L范围内线性关系良好（r≥0.99）。方法的定量限（S/N=10）为5.0 μg/kg，在5.0、10.0、20.0 μg/kg的添加浓度的回收率为61.2%~108.5%，相对标准偏差（RSD，n=6）为1.1%~9.8%。该方法快速、灵敏、准确，适合于多种基质中磺胺增效剂的测定。

关键词: 超高效液相色谱-串联质谱, 动物源性食品, 磺胺增效剂

Abstract:

A method for the determination of sulfonamide potentiators, trimethoprim (TMP), diaveridine (DVD) and ormetoprin (OMP), in different animal origin food matrices (including chicken muscle, fish muscle, chicken liver, egg and milk) has been developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted by formic acid-acetonitrile (1:9, v/v), cleaned-up by hexane, separated on an Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution. The determination was carried out with electrospray ion source under the positive mode and multiple reaction monitoring (MRM) mode. The extraction recoveries of three extraction solvents were observed. The purification condition and concentration condition were optimized. In addition, the mobile phase, column temperature and solid phase extraction column were studied. The calibration curves showed a good linearity in the range of 1.25-30.0 μg/L, and the correlation coefficients (r) were higher than 0.99. The limits of quantification (LOQ, S/N=10) of the three potentiators were 5.0 μg/kg. At the spiked levels of 5.0, 10.0 and 20.0 μg/kg, the recoveries of the three potentiators were ranged from 61.2% to 108.5%, and the relative standard deviations (RSD, n=6) ranged from 1.1% to 9.8%. The results indicate that the method is simple, rapid, sensitive and suitable for the qualitative and quantitative analysis of the three potentiators in multiple matrices.

Key words: animal origin foods, sulfonamide potentiators, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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