超高效液相色谱-串联质谱法检测水产品中10种氨基糖苷类药物残留  

Simultaneous Determination of 10 Kinds ofAminoglycosides inAquatic Products by Ultra Performance Liquid Chromatography-TandemMass Spectrometry

作　　者：李佩佩[1] 何鹏飞 严忠雍[1] 方益[1] LI Pei-pei;HE Peng-fei;YAN Zhong-yong;FANG Yi(Laboratory of Aquatic Product Processing and Quality Safety,Marine Fisheries Research Institute of Zhejiang/Key Lab of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang Province,Zhoushan 316021,China)

机构地区：[1]浙江省海洋水产研究所水产品加工与质量安全研究室/浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江舟山316021

出　　处：《广东海洋大学学报》2023年第2期104-112,共9页Journal of Guangdong Ocean University

基　　金：浙江省科技计划项目(LGC22B050032,LGN22C200018)。

摘　　要：【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、10.0μg/kg,潮霉素B和安普霉素的检出限和定量限分别为2.0、5.0μg/kg,其余7种氨基糖苷类药物的检出限和定量限分别为1.0μg/kg和2.0μg/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 5.0μg/kg and 10.0μg/kg,respectively;LOD and LOQ of hygromycin B and apramycin were 2.0μg/kg and 5.0μg/kg,respectively;LOD and LOQ of the other 7 kinds AGs were 1.0μg/kg and 2.0μg/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.

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 

分 类 号：O657.63[理学—分析化学]