色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-电喷雾串联质谱法测定蜂蜜中的林可胺类抗生素残留

徐锦忠,吴斌,丁涛,沈崇钰,赵增运,陈惠兰,蒋原

  

  1. National Bee-Product Reference Laboratory, Animal, Plant and Food Inspection Center (APFIC) of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • 收稿日期:2005-11-15 修回日期:2006-06-12 出版日期:2006-09-30 发布日期:1986-09-25
  • 通讯作者: 徐锦忠

Determination of Lincosamide Residues in Honey Using High Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

XU Jinzhong, WU Bin, DING Tao, SHEN Chongyu, ZHAO Zengyun, CHEN Huilan, JIANG Yuan   

  1. National Bee-Product Reference Laboratory, Animal, Plant and Food Inspection Center (APFIC) of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2005-11-15 Revised:2006-06-12 Online:2006-09-30 Published:1986-09-25

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摘要：

建立了蜂蜜中林可胺类抗生素林可霉素和氯林可霉素的高效液相色谱-电喷雾串联质谱(HPLC/ESI-MS/MS)检测方法。样品经固相萃取提取净化、反相液相色谱分离后进行质谱分析,在选择反应监测模式(SRM) 下进行特征母-子离子对信号采集。根据保留时间、母离子和两个特征子离子信息进行定性分析,以共同的基峰离子m/z 126进行定量。两种抗生素的检测限(S/N=3) 为 0.1 μg/kg,定量限为 0.5 μg/kg,在1.0～200 μg/L时峰强度与质量浓度的线性关系良好(r2>0.996)。在1.0,5.0,20.0 μg/kg 3个添加水平,两种抗生素的平均回收率范围为80%～110%,日内测定结果的相对标准偏差小于8%,日间测定结果的相对标准偏差小于15%。结果表明,该法简单、灵敏,特异性强,适用于蜂蜜中林可胺类抗生素残留的分析确证。

关键词: 电喷雾串联质谱, 蜂蜜 , 高效液相色谱, 林可胺类抗生素, 林可霉素, 氯林可霉素

Abstract:

An analytical method for the determination of lincosamide antibiotic residues in honey was developed. In the procedure a solid-phase extraction for the isolation of lincomycin and clindamycin from diluted honey samples was employed. The residues of lincomycin and clindamycin were subsequently analyzed by reversed-phase high performance liquid chromatography (RP-HPLC) coupled with electrospray tandem mass spectrometry. Mass spectral acquisition was applied with selective reaction monitoring of two diagnostic transition reactions. The qualitative analysis was based on the retention time, the precursor ion and two product ions, and the quantitation was carried out with intension of the characteristic ion m/z 126. The linear ranges were from 1.0 μg/L to 200 μg/L for lincomycin and clindamycin and the correlation coefficients (r2) were all greater than 0.996. The average recoveries for lincomycin and clindamycin ranged from 80% to 110% in replicate sets of honey samples spiked with the drug concentrations of 1.0, 5.0 and 20.0 μg/kg, and the relative standard deviations (RSDs) were less than 8% for intra-day and 15% for inter-day determinations. The method detection limit and quantitation limit were 0.1 μg/kg and 0.5 μg/kg, respectively. The method is simple and suitable for routine analysis.

Key words: clindamycin, electrospray tandem mass spectrometry （ESI-MS/MS), honey , lincomycin, lincosamide antibiotics, high performance liquid chromatography (HPLC)