色谱

色谱 ›› 2012, Vol. 30 ›› Issue (11): 1143-1147.DOI: 10.3724/SP.J.1123.2012.06024

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法检测乳制品中10种氨基糖苷类抗生素残留

龚强, 丁利, 朱绍华, 焦艳娜, 成婧, 付善良, 王利兵*   

  1. 湖南出入境检验检疫局技术中心, 食品安全科学技术湖南省重点实验室, 湖南 长沙 410004
  • 收稿日期:2012-06-20 修回日期:2012-09-27 出版日期:2012-11-28 发布日期:2012-11-21
  • 通讯作者: 王利兵,博士,研究员,研究方向为食品安全与检验检疫安全. Tel: (0731)85627689, E-mail: wanglb1@163.com.
  • 基金资助:

    国家“十二五”科技支撑计划项目(2011BAK10B05, 2012BAD29B05).

Determination of ten aminoglycoside residues in milk and dairy products using high performance liquid chromatography-tandem mass spectrometry

GONG Qiang, DING Li, ZHU Shaohua, JIAO Yanna, CHENG Jing, FU Shanliang, WANG Libing*   

  1. Technology Center of Hunan Entry-Exit Inspection and Quarantine Bureau, Hunan Key Laboratory of Food Safety Science & Technology, Changsha 410004, China
  • Received:2012-06-20 Revised:2012-09-27 Online:2012-11-28 Published:2012-11-21

PDF

708

被引次数

33

摘要： 建立了乳制品中链霉素、双氢链霉素、新霉素、卡那霉素、妥布霉素、庆大霉素、安普霉素、潮霉素B、巴龙霉素、阿米卡星等10种氨基糖苷类抗生素(aminoglycosides, AGs)残留的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。乳制品提取液经亲水-亲脂平衡(hydrophilic- lipophilic balance, HLB)柱净化后,采用反相离子对高效液相色谱分离,电喷雾串联四极杆质谱检测。对样品前处理条件、液相色谱流动相以及质谱条件进行了优化。结果表明: 10种AGs在20～1000 μg/L范围内定量离子的峰面积和样品的质量浓度之间有很好的线性关系;在乳制品中的加标回收率为71.2%～101.7%,相对标准偏差为3.4%～13.8%。该方法简便、灵敏、准确,可用于乳制品中多种AGs残留的同时检测。

关键词: 氨基糖苷类抗生素, 高效液相色谱-串联质谱, 亲水-亲脂平衡柱, 乳制品

Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analytical method was developed for the simultaneous determination of ten aminoglycoside residues (streptomycin, dihydrostrepmycin, neomycin, kanamycin, tobramycin, gentamycin, apramycin, hygromycin B, paromomycin, and amkacin) in milk and dairy products. The sample was extracted with 5% trichloroacetic acid aqueous solution, then the extract was purified by a hydrophilic-lipophilic balance (HLB) cartridge. The ten aminoglycoside residues were separated by ion-pair reversed phase high performance liquid chromatography. Heptafluorobutyric acid was used as ion pair agent due to its volatility. Then the analytes were detected by electrospray ionization tandem mass spectrometry. The pretreatment condition of the sample, the HPLC condition and the MS operation parameters were optimized. The results showed that the linearities of the ten aminoglycoside residues in 20~1000 μg/L had the correlation coefficient between 0.9946~0.9997. The recoveries ranged from 71.2% and 101.7% with the relative standard deviations of 3.4%~13.8%. The proposed method was successfully applied to the determination of the mass concentrations of the analytes in related samples, which provides a simple, and convenient method for the quality control of milk and dairy products. Furthermore, this method is effective for the safety monitoring of aminoglycoside residues in milk and dairy products.

Key words: aminoglycosides, hydrophilic-lipophilic balance (HLB) cartridge, milk and dairy products, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

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