摘要
目的:建立一种UPLC-MS/MS同时检测淡水鱼中16种喹诺酮类抗生素的方法,并分析水煮、清蒸及油炸3种不同烹饪方式对喹诺酮类抗生素残留量的影响。方法:样品经乙腈(含4%甲酸)超声提取,C_(18)固相萃取柱净化,Waters ACQUITY UPLC BEH C_(18)(1.7μm,2.1 mm×100 mm)色谱柱分离,以0.1%甲酸水—乙腈为流动相梯度洗脱。质谱(ESI+)采用多反应离子监测模式,内标法定量。结果:在2.0~50.0 ng/mL质量浓度范围内,16种喹诺酮类抗生素呈良好线性关系,相关系数>0.99849,检出限和定量限分别为0.3~4.1,0.9~11.0μg/kg;基质中低、中、高3个添加水平下的平均回收率为79.0%~104.7%,相对标准偏差为1.0%~8.1%;与对照相比,3种不同烹饪方式的鱼肉阳性样品中16种喹诺酮类抗生素残留量均无显著性差异。结论:该方法前处理简便快速、灵敏度高,能够满足淡水鱼中多种喹诺酮类抗生素的高通量筛查及膳食风险评价。
Objective:This study aimed to establish a method for the simultaneous determination of 16 quinolones in freshwater fish by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)and then analyze the effect of three different cooking methods(by boiling,steaming and frying)on the residues of quinolone antibiotics.Methods:Samples were ultrasonic extracted with acetonitrile(with 4%formic acid)and purified with C_(18) solid phase extraction column.The chromatographic separation was performed on a Waters ACQUITY UPLC BEH C_(18)(1.7μm,2.1 mm×100 mm)column,with 0.1%formic acid water-acetonitrile as mobile phase for gradient elution.Mass spectrometry(ESI+)was monitored by multiple reaction ions and quantified by internal standard method.Results:16 quinolones showed a clear linear relationship between 2.0 ng/mL and 50 ng/mL,and the correlation coefficient was greater than 0.99849.The limits of detection quantification were 0.3~4.1μg/kg and 0.9~11.0μg/kg,respectively.Average recoveries in matrices at low,medium,and high spiked levels ranged from 79.0%to 104.7%,with a standard deviation of 1.0%to 8.1%.There was no significant difference in the residues of 16 quinolones between the fish meat-positive samples of three different cooking methods and the control.Conclusion:The method was simple,rapid,and sensitive,and met the high-throughput screening and dietary risk assessment of quinolone antibiotics in freshwater fish.
作者
高云慨
陈春泉
陈小妹
周凌聿
邓英林
尹青春
GAO Yunkai;CHENG Chunqian;CHENG Xiaomei;ZHOU Lingyu;DEND Yinglin;YIN Qingchun(Hainan Institute for Food Control,Key Laboratory of Tropical Fruits and Vegetables Quality Safety for State Market Regulation,Haikou,Hainan 570100,China)
出处
《食品与机械》
CSCD
北大核心
2024年第1期40-46,54,共8页
Food and Machinery
基金
国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(编号:ZZ-2022001)。
作者简介
高云慨,男,海南省食品检验检测中心中级工程师,硕士;通信作者:尹青春(1986-),女,海南省食品检验检测中心高级工程师,硕士。E-mail:yinqingchun@163.com。
