色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 519-523.DOI: 10.3724/SP.J.1123.2013.12028

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法检测牛奶中头孢洛宁残留

李帅鹏1, 郭春娜1, 孟蕾2, 黄显会1   

  1. 1. 华南农业大学国家兽药残留基准实验室, 广东 广州 510642;
    2. 河南省兽药监察所, 河南 郑州 450008
  • 收稿日期:2013-12-25 修回日期:2014-02-27 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 黄显会
  • 基金资助:

    公益性行业（农业）科研专项（201303038-5）.

Determination of cefalonium residue in milk by high performance liquid chromatography-tandem mass spectrometry

LI Shuaipeng1, GUO Chunna1, MENG Lei2, HUANG Xianhui1   

  1. 1. National Reference Laboratory of Veterinary Drug Residues, South China Agricultural University, Guangzhou 510642, China;
    2. Henan Institute of Veterinary Drug Control, Zhengzhou 450008, China
  • Received:2013-12-25 Revised:2014-02-27 Online:2014-05-08 Published:2014-04-26

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摘要：

建立了牛奶中头孢洛宁残留检测的高效液相色谱-串联质谱方法。1 g牛奶经乙腈沉淀蛋白质后，上清液于37 ℃水浴下氮气吹干，用1 mL甲醇-0.1%甲酸水溶液（3：7，v/v）复溶，正己烷除脂净化后检测。流动相为乙腈和0.1%甲酸水溶液，梯度洗脱，经C18色谱柱分离，采用多反应监测正离子模式对头孢洛宁进行定性定量分析。采用基质匹配法对牛奶中头孢洛宁的含量进行标准校正，在2~200 μg/L范围内，头孢洛宁质量浓度与其对应峰面积的线性关系良好，相关系数>0.999。牛奶中加标样品的检出限（按S/N≥3计）为0.5 μg/kg，定量限（S/N≥10计）为2 μg/kg。在定量限、1/2最高残留限量、最高残留限量、2倍最高残留限量添加水平下，牛奶中头孢洛宁的平均回收率为78.5%~86.2%，日内相对标准偏差为1.5%~6.2%，日间相对标准偏差为2.9%~5.6%。该方法可用于牛奶中头孢洛宁的残留检测。

关键词: 残留, 串联质谱, 高效液相色谱, 牛奶, 头孢洛宁

Abstract:

An analytical method was developed for the determination of cefalonium in milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A total of 1 g milk was deproteinized by acetonitrile. The supernatant was transferred into a test tube to be blown dry with N2 at 37 ℃. Then the residue was dissolved with methanol-0.1% formic acid in water (3:7, v/v). The sample was determined by HPLC-MS/MS after the purification. The chromatographic separation was achieved on a C18 column using 0.1% formic acid in water and acetonitrile as mobile phases with gradient elution. Qualitative and quantitative analyses were achieved by HPLC-MS/MS under positive ionization and multiple reaction monitoring (MRM) mode. Matrix-matched calibration curve was used for the quantification. Good correlation coefficients were obtained (r>0.999) in the mass concentration range of 2-200 μg/L. The limit of detection (LOD, S/N≥3) was 0.5 μg/kg in milk, and the limit of quantification (LOQ, S/N≥10) was 2 μg/kg. The mean recoveries at the four levels of LOQ, 1/2MRL (maximum residue level), MRL, 2MRL were between 78.5% and 86.2%, with the intra-day relative standard deviations (RSDs)of 1.5% to 6.2% and inter-day RSDs of 2.9% to 5.6%. In conclusion, the established method can be applied for the determination of cefalonium residue in milk.

Key words: cefalonium, high performance liquid chromatography (HPLC), milk, residue, tandem mass spectrometry (MS/MS)

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