色谱

色谱 ›› 2019, Vol. 37 ›› Issue (5): 499-504.DOI: 10.3724/SP.J.1123.2018.11043

• 研究论文 • 上一篇    下一篇

混合型离子交换液相色谱-串联质谱法测定蜂蜜中5种氨基糖苷类抗生素残留

吴云辉2, 严丽娟1, 沈鹭英1, 林立毅1, 张峰3, 徐敦明1   

  1. 1. 厦门海关检验检疫技术中心, 福建 厦门 361026;
    2. 厦门海洋职业技术学院, 福建 厦门 361100;
    3. 中国检验检疫科学研究院, 北京 100176
  • 收稿日期:2018-12-05 出版日期:2019-05-08 发布日期:2015-03-23
  • 通讯作者: 徐敦明,Tel:(0592)7250900,E-mail:Dunmingxu@163.com
  • 基金资助:

    国家重点研发计划项目（2017YFC1601600）；福建省自然科学基金（2016J01071）；原国家质检总局项目（2016IK184）；厦门市科技惠民项目（3502Z20174040，3502Z20174043）.

Determination of five aminoglycoside residues in honey using mixed-mode ion exchange liquid chromatography-tandem mass spectrometry

WU Yunhui2, YAN Lijuan1, SHEN Luying1, LIN Liyi1, ZHANG Feng3, XU Dunming1   

  1. 1. Inspection and Quarantine Technology Center, Xiamen Customs, Xiamen 361026, China;
    2. Xiamen Ocean Vocational College, Xiamen 361100, China;
    3. Chinese Academy of Inspection and Quarantine, Beijing 100176, China
  • Received:2018-12-05 Online:2019-05-08 Published:2015-03-23
  • Supported by:

    National Key Research and Development Program of China (No. 2017YFC1601600); Natural Science Foundation of Fujian Province (No. 2016J01071); Former General Administration of Quality Supervision, Inspection and Quarantine Project (No. 2016IK184); Science and Technology People-Benefit Project of Xiamen (Nos. 3502Z20174040, 3502Z20174043).

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摘要：

建立了混合型离子交换液相色谱-串联质谱测定蜂蜜中链霉素、双氢链霉素、壮观霉素、卡那霉素和阿米卡星等5种氨基糖苷类抗生素的方法。蜂蜜样品采用磷酸盐缓冲溶液提取，分子印迹固相萃取柱富集净化，Obelisc R色谱柱分离，以0.1%（v/v）甲酸水溶液和乙腈为流动相进行梯度洗脱，采用电喷雾电离、正离子模式扫描，多反应监测模式检测，外标法定量。实验结果表明，链霉素和双氢链霉素在5~100 μg/L范围内呈现良好的线性关系，定量限为5 μg/kg；壮观霉素、卡那霉素和阿米卡星在20~500 μg/L范围内呈现良好的线性关系，定量限为20 μg/kg。在空白蜂蜜样品中添加1倍、2倍和5倍定量限水平的5种氨基糖苷类药物，其平均回收率为75.1%~92.3%，相对标准偏差为4.5%~10.7%。该法不添加离子对试剂，可减少对质谱仪的污染，并具有较高的灵敏度，适用于蜂蜜中5种氨基糖苷类抗生素的同时检测。

关键词: 氨基糖苷类抗生素, 蜂蜜, 混合型离子交换液相色谱-串联质谱

Abstract:

A method using mixed-mode ion exchange liquid chromatography-tandem mass spectrometry was developed for the determination of streptomycin, dihydrostreptomycin, spectinomycin, kanamycin and amikacin in honey. The honey samples were extracted with phosphate followed by clean-up with SupelMIP Aminoglycosides SPE cartridges. The separation was performed on an SIELC Obelisc R column (100 mm×2.1 mm, 5 μm) by the gradient elution program using 0.1%(v/v) formic acid aqueous solution and acetonitrile as the mobile phases, at a flow rate of 0.4 mL/min. Five aminoglycosides (AGs) were identified by the tandem mass spectrometer with an electrospray ionization source under the multiple reaction monitoring (MRM) mode. The quantification analysis was performed by the external standard method. The calibration curves showed good linearity in the range of 5-100 μg/L for streptomycin and dihydrostreptomycin, and 20-500 μg/L for spectinomycin, kanamycin and amikacin. The limits of quantification (LOQs) of the five drugs in honey were 5-20 μg/kg. The average recoveries of the five drugs from feeds spiked at LOQ, 2-fold LOQ and 5-fold LOQ levels were 75.1%-92.3%, and the relative standard deviations (RSDs) were 4.5%-10.7%. The method is simple, rapid, and sensitive, and is suitable for the simultaneous determination of the five aminoglycoside residues in honey.

Key words: aminoglycoside, honey, mixed-mode ion exchange liquid chromatography-tandem mass spectrometry

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