摘要
建立了QuEChERS净化结合超高效液相色谱串联四级杆飞行时间质谱(UHPLC-Q-TOF/MS)法同时筛查猪肉中10种抗生素类兽药残留量的分析方法。样品经过Na;EDTA-Mcllvaine缓冲溶液-0.1%甲酸乙腈-NaCl-无水Na_(2)SO_(4)-C_(18)的提取净化。通过Infinity Lab Poroshell 120 EC-C_(18)色谱柱分离,在正离子多反应监测模式下分析。结果表明,10种兽药相关系数大于0.99,在5.0~100.0μg/kg范围内线性关系良好,在5、10、20μg/kg三个添加水平下平均回收率为72.3%~117.3%,日内相对标准偏差为(Relative Standard Deviation,RSD)0.9%~10.4%,日间RSD为1.1%~13.4%,检测限(Limit of Detection,LOD)为0.25~1.0μg/kg,定量限(Limit of Quantity,LOQ)为0.5~5.0μg/kg。采用本方法对市场购买的50份新鲜生猪肉样品进行检测,1份样品四环素呈阳性,其余样品均未检出。该方法操作简便、快速,具有良好的精密度和定量限,适用于猪肉中10种抗生素类兽药的快速检测。
A method for simultaneous determination of 10 veterinary antibiotics residues in pork by QuEChERS purification combined with ultra performance liquid chromatography tandem quadrupole-time of flight mass spectrometry(UHPLC-Q-TOF/MS) was developed. The sample was extracted and purified by Na;EDTA-Mcllvaine buffer solution-0.1%formic acid acetonitrile-NaCl-anhydrous Na_(2)SO_(4)-C_(18). The separation was performed on an Infinity Lab Poroshell 120 EC C_(18) column and analyzed under the positive ion multi-reaction monitoring mode. The results showed that the correlation coefficients of 10 veterinary drugs were greater than 0.99, and the linear range was 5.0~100.0 μg/kg. The average recoveries were 72.3%~117.3% at the spiked levels of 5, 10, 20 μg/kg. The intra-day relative standard deviations(RSD) was 0.9% to10.4%, and the within-day RSD was 1.1% to 13.4%. The limit of detection(LOD) was 0.25~1.0 μg/kg, and the limit of quantification(LOQ) was 0.5~5 μg/kg. This method was used to detect 50 fresh raw pork samples purchased in the market.One sample was positive for tetracycline, and none of the other samples were detected. The method was simple and fast to operate, had good precision and limit of quantification, and was suitable for the rapid detection of 10 antibiotic veterinary drugs in pork.
作者
裴斐
韩萍
王杰
马宁
苏安祥
杨文建
胡秋辉
PEI Fei;HAN Ping;WANG Jie;MA Ning;SU Anxiang;YANG Wenjian;HU Qiuhui(College of Food Science and Engineering,Nanjing University of Finance and Economics,Jiangsu Key Laboratory of Grain and Oil Quality Control and Deep Processing,Jiangsu Collaborative Innovation Center for Modern Grain Circulation and Safety,Nanjing 210023,China)
出处
《食品工业科技》
CAS
北大核心
2022年第10期298-304,共7页
Science and Technology of Food Industry
基金
江苏高校“青蓝工程”资助项目
江苏省高校优势学科建设工程资助项目(PAPD)。
