栾枫婷 龚兰 朱磊 陈明 唐敏敏 邵雪梅 魏瑞成 王冉

摘要： 建立了高效液相色谱-串联质谱法测定蛋和奶中氨基糖苷类药物（双氢链霉素、卡那霉素A、庆大霉素、链霉素、妥布霉素、潮霉素B、大观霉素、阿米卡星、新霉素B和安普霉素）残留。用5%三氯乙酸水溶液提取目标物，经HLB固相萃取柱净化，高效液相色谱柱分离，梯度洗脱，外标法定量。结果表明，10种药物在各自范围内线性关系良好，R2>0.99，方法的检出限为10.0～50.0 μg/kg，定量限为30.0～100.0 μg/kg，平均回收率为62.3%～110.4%，相对标准偏差为1.0%～13.6%。该方法简便、准确、灵敏，且扩大了检测范围，适用于蛋和奶中氨基糖苷类药物的定量测定。

关键词： 高效液相色谱-串联质谱;固相萃取;氨基糖苷类药物;残留;禽蛋;奶

中图分类号： S859.84   文献标识码： A   文章编号： 1000-4440（2021）04-1033-10

Determination of aminoglycoside residues in eggs and milk by high-performance liquid chromatography-tandem mass spectrometry

LUAN Feng-ting1，2， GONG Lan1，2， ZHU Lei1，2， CHEN Ming1，2， TANG Min-min1，2， SHAO Xue-mei1，2，WEI Rui-cheng1，2， WANG Ran1，2

（1.Key Lab of Food Quality and Safety of Jiangsu Province-State Key Laboratory Breeding Base， Nanjing 210014， China;2.Institute of Food Safety and Nutrition， Jiangsu Academy of Agricultural Sciences， Nanjing 210014， China）

Abstract： The high-performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was developed for the simultaneous determination of ten aminoglycosides （dihydrostreptomycin， kanamycin A， gentamycin， streptomycin， spectinomycin， tobramycin， hygromycin B， amikacin， neomycin B and apramycin） in milk and eggs. The samples were extracted with 5% trichloroacetic acid solution， followed by Oasis HLB solid phase extraction for further purification. The analytes were separated on a high performance liquid chromatography column， then analyzed by MS/MS with electrospray ionization in positive mode， and quantified by external standard method. Results showed that there were good linear relationships for 10 target analytes， and the linear correlation coefficients were greater than 0.99. The limits of detection and the limits of quantitation were in the ranges of 10.0-50.0 μg/kg and 30.0-100.0 μg/kg， respectively. The average recoveries for ten aminoglycosides ranged from 62.3% to 110.4% with relative standard deviations of 1.0%-13.6%. The developed method is simple， rapid， accurate， sensitive and has wide detection range， so it is suitable for the determination of ten aminoglycosides in eggs and milk.

Key words： high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）;solid phase extraction （SPE）;aminoglycosides （AGs）;residues;eggs;milk

氨基糖苷類药物（Aminoglycosides，AGs）是通过氨基糖和氨基环醇以苷键结合而构成，主要作用是阻碍细菌的蛋白质合成，使细菌细胞壁的通透性发生变化，从而发挥抗菌作用。AGs因其价格低廉且具有广谱抗菌性，被广泛用于治疗和预防禽霍乱、奶牛乳腺炎及奶牛结核病等，还作为促生长剂提高饲料报酬率[1]。但该类药物长期食用后易蓄积于动物细胞、组织和器官中，食用这些动物产品后会损害人体健康。近年来，有文献报道AGs对人体具有显著的耳毒性、肾毒性且会损害前庭神经功能，严重时会导致休克，甚至死亡[2]。由农业农村部、国家卫生健康委员会和国家市场监督管理总局联合发布的食品安全国家标准《食品中兽药最大残留限量……