摘要
为有效筛查牛乳中抗生素残留风险以确保消费者安全,采用改进的PRiME HLB固相萃取联合高效液相色谱法同时检测牛乳中5种限用氟喹诺酮类药物残留。利用Box-Behnken统计设计进行响应面优化,样品经0.5%甲酸乙腈溶液萃取后,以Oasis PRiME HLB SPE柱净化;并以乙腈和0.1%甲酸溶液为流动相,利用Ultimate XB C_(18)色谱柱(250 mm×4.6 mm,5 μm)进行分离检测,外标法定量。结果表明:5种氟喹诺酮类药物在线性范围内线性良好,相关系数(R2)均大于0.991;方法检测限在1.0~4.0 μg/kg,定量限在2.0~13.0 μg/kg;回收率为93.0%~114.2%,RSD均小于8.8%。可应用于保障牛乳中氟喹诺酮类药物残留质量安全。
To effectively screen the risk of antibiotics residues in milk to ensure consumer safety,a pass-through solid-phase extraction purification with high-performance liquid chromatography method for the determination of five restricted fluoroquinolones in milk was developed.Compounds were extracted by 0.5% acidified acetonitrile,and purified by Oasis PRiME HLB SPE column,five fluoroquinolones were separated by Ultimate XB C_(18) column (250 mm×4.6 mm,5 μm) using acetonitrile and 0.1% formic acid as mobile phases,then were quantified by external standard method.The results showed that this method exhibited a good linearity for analytes with R2﹥0.991 in their standard calibration curves.The limits of determination (LODs) and the limits of quantification (LOQs) were 1.0~4.0 μg/kg and 2.0~13.0 μg/kg,respectively,and recoveries in milk ranged from 93.0% to 114.2%,with the relative standard deviations (RSDs)≤8.8%,respectively.This method can be applied to ensure the safety of fluoroquinolones residues in milk.
作者
彭大红
梅艳珍
郝爱月
戴传超
PENG Dahong;MEI Yanzhen;HAO Aiyue;DAI Chuanchao(Jiangsu Engineering and Technology Research Center for Industrialization of Microbial Resources,Jiangsu Key Laboratory for Microbes and Functional Genomics,College of Life Sciences,Nanjing Normal University,Nanjing 210023,China)
出处
《食品科技》
CAS
北大核心
2021年第8期276-283,共8页
Food Science and Technology
基金
国家重点研发计划项目(2018YFC1600476)。
