2023, 43(2): 104-112. doi: 10.3969/j.issn.1673-9159.2023.02.013
关键词： 水产品 , 氨基糖苷类药物 , 药物残留检测 , 超高效液相色谱-串联质谱
Keywords： aquatic products , aminoglycosides , simultaneous determination , ultra performance liquid chromatography-tandem mass spectrometry
【目的】建立同时检测水产品中壮观霉素、潮霉素B、双氢链霉素、链霉素、丁胺卡那霉素、卡那霉素、安普霉素、妥布霉素、庆大霉素、新霉素等10种氨基糖苷类药物的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。【方法】样品用10 mmol/L磷酸二氢钾缓冲溶液提取，用氢氧化钠溶液将提取液的pH调为6.6~7.0，取一半体积提取液上HLB固相萃取柱净化，采用Obelisc R柱高效分离，电喷雾正离子多反应监测模式监测。【结果与结论】10种氨基糖苷类药物呈现良好的线性关系（R2> 0.999），新霉素的检出限和定量限分别为5.0、10.0 μg/kg，潮霉素B和安普霉素的检出限和定量限分别为2.0、5.0 μg/kg，其余7种氨基糖苷类药物的检出限和定量限分别为1.0 μg/kg和2.0 μg/kg。10种分析物的加标回收率为74.8%~104.5%，相对标准偏差（RSD）为4.5%~12.6%。本方法分析时间短，5 min内即完成10种药物的分离，分析物峰形尖锐。方法灵敏度、准确度高，适用于水产品中10种氨基糖苷类药物的同时测定。
【Objective】An ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of 10 kinds of aminoglycosides (AGs), including spectinomycin, hygromycin B, dihydrostrepmycin, streptomycin, amikacin, kanamycin, apramycin, tobramycin, gentamycin and neomycin in edible parts of aquatic products. 【Method】The samples were extracted with 10 mmol/L potassium dihydrogen phosphate buffer solution, then the pH of the extract was adjusted to be neutral by sodium hydroxide. Half of the volume was cleaned-up and pre-concentrated using Hydrophile Lipophilic Balance (HLB) cartridge. All the target compounds were separated on an Obelisc R column and detected by UPLC-MS/MS under ESI + ionization Multiple response monitoring (MRM) mode. 【Result and Conclusion】 Under optimized conditions, this method had a good linearity (R2>0.999). The limit of detection (LOD, S/N≥ 3) and the limits of quantification (LOQ, S/N≥10) of neomycin were 5.0 μg/kg and 10.0 μg/kg, respectively; LOD and LOQ of hygromycin B and apramycin were 2.0 μg/kg and 5.0 μg/kg, respectively; LOD and LOQ of the other 7 kinds AGs were 1.0 μg/kg and 2.0 μg/kg, respectively. Besides, the average recoveries presented 78.4%-104.5% with the relative standard deviations (RSDs, n = 6) of 4.5%-12.6%. The analysis was rapid and can be achieved in less than 5 min. The method had the characteristics of high accuracy and good precision, was suitable for simultaneous determination of 10 kinds of AGs in aquatic products.
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