Detection of 10 Aminoglycosides Drugs in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry

SUN Ting; SHEN Lu-ying; HE Jin-lin; ZHAN Yong-chao; YAN Li-juan; XU Dun-ming

doi:10.12452/j.fxcsxb.24032603

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Detection of 10 Aminoglycosides Drugs in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2024-07-08

- Detection of 10 Aminoglycosides Drugs in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 43, Issue 7, Pages: 1046-1051(2024)
- 作者机构：
  
  厦门海关技术中心，福建厦门 361026
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.24032603
  CLC： O657.7;TS207.3
- Published：15 July 2024，
  
  Received：26 March 2024，
  
  Revised：11 May 2024，
- 稿件说明：
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孙婷,沈鹭英,何金麟,占永超,严丽娟,徐敦明.高效液相色谱-串联质谱法测定蜂蜜中10种氨基糖苷类药物[J].分析测试学报,2024,43(07):1046-1051.

SUN Ting,SHEN Lu-ying,HE Jin-lin,ZHAN Yong-chao,YAN Li-juan,XU Dun-ming.Detection of 10 Aminoglycosides Drugs in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(07):1046-1051.
孙婷,沈鹭英,何金麟,占永超,严丽娟,徐敦明.高效液相色谱-串联质谱法测定蜂蜜中10种氨基糖苷类药物[J].分析测试学报,2024,43(07):1046-1051. DOI： 10.12452/j.fxcsxb.24032603.

SUN Ting,SHEN Lu-ying,HE Jin-lin,ZHAN Yong-chao,YAN Li-juan,XU Dun-ming.Detection of 10 Aminoglycosides Drugs in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(07):1046-1051. DOI： 10.12452/j.fxcsxb.24032603.

摘要

建立了高效液相色谱-串联质谱（HPLC-MS/MS）检测蜂蜜中10种氨基糖苷类药物（安普霉素、庆大霉素C

、卡那霉素、潮霉素B、巴龙霉素、阿米卡星、依替米星、奈替米星、妥布霉素和核糖霉素）残留量的方法。蜂蜜样品采用100 mmol/L磷酸盐缓冲液（pH 8.0）提取，SupelMIP SPE-Aminoglycosides分子印迹聚合物固相萃取柱净化，Thermo Hypercarb色谱柱分离，以 5%氨水和乙腈为流动相进行梯度洗脱，采用HPLC-MS/MS电喷雾正离子模式检测，基质匹配标准曲线外标法定量。结果表明，10种氨基糖苷类药物在20~500 μg/L范围内线性关系良好，方法定量下限为25 μg/kg。在25、50、250 μg/kg 3个加标水平下，10种氨基糖苷类药物的平均回收率为73.4%～93.2%，相对标准偏差（RSD）为5.2%～11%。该方法简便、灵敏度高，无需离子对试剂，有效减少了对质谱仪的污染，能够较好地满足蜂蜜中氨基糖苷类药物残留量的检测需要。

Abstract

A method was established for the detection of residues of ten aminoglycoside（AGs） drugs（apramycin，gentamycin C

，kanamycin，hygromycin B，paromomycin，amikacin，etimicin，netimicin，tobramycin and ribostamycin） in honey using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. Several conditions were optimized，including sample extraction and purification，chromatographic conditions and mass spectrometry parameters.The honey samples were extracted with 100 mmol/L phosphate buffer（pH 8.0） and purified with SuperMIP SPE column. The eluent was 1.0 mL acetonitrile water（20∶80，volume ratio） solution containing 5% formic acid. Further

more，the chromatographic separation conditions and response intensities of the 10 AGs in different mobile phases were compared. The optimized HPLC conditions were as follows：Thermo Hypercarb chromatography column（150 mm×2.1 mm，5 μm）；column temperature，35 ℃；flow rate，0.35 mL/min；injection volume，10 μL；mobile phase A：5% ammonia solution；mobile phase B：acetonitrile. The samples were quantified using positive-ion multiple reaction monitoring（MRM） mode for 13 min. The AGs were quantified using an external standard with matrix calibration curves to reduce the influences of the matrix effects on the quantitative results. The calibration curves showed good linearity in the range of 20-500 μg/L，and the limits of quantification（LOQs） of ten aminoglycoside drugs in honey were 25 μg/kg. The recoveries for the analytes at three spiked levels（25，50，250 μg/kg） ranged from 73.4% to 93.2%，with relative standard deviations（RSDs）of 5.2%-11%. The method is simple，highly sensitive，and avoids the use of ion pair reagents throughout the process，effectively reducing contamination of the mass spectrometer and it is suitable for detection of aminoglycosides in honey.

关键词

氨基糖苷类药物高效液相色谱-串联质谱分子印迹固相萃取蜂蜜

Keywords

aminoglycosides drugshigh performance liquid chromatography-tandem mass spectrometryMIP-SPEhoney

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