HPLC-MS同时检测牛奶中喹诺酮和磺胺类药物的残留
Simultaneous detection of quinolone and sulfonamide residues in milk by HPLC-MS
王军锋 1李安 1庞兴萍 1曹文玉 1闫璐璐1
作者信息
- 1. 陕西学前师范学院化学化工学院,陕西西安 710100
- 折叠
摘要
目的为确保牛奶质量,建立HPLC-MS检测牛奶中两种喹诺酮类药物恩诺沙星(ENR)、诺氟沙星(NOR)和1种磺胺类药物磺胺嘧啶(SD)残留量的实验方法.方法水相为0.1％甲酸水溶液,有机相为0.1％甲酸乙腈,优化质谱、色谱条件,外标法定量.结果混合标准品中ENR在10.00～100.0ng·mL-1浓度区间内、NOR在10.00～150.00ng·mL-1浓度区间内、SD在20.00～250.00ng·mL-1浓度区间内均具有良好的线性关系,R2分别为 0.988、0.944、0.947.在 ENR、NOR、SD 加标浓度为 25、100、100ng·mL-1 的水平下,回收率均在 90％～105％范围内,相对标准偏差(RSD,n=12)分别为16％、9.4％、9.6％,方法检出限为8.48、2.09、1.87ng·mL-1,定量限为9.94、9.78、15.35ng·mL-1.结论该方法具有灵敏度高和选择性强等优点,适合牛奶中喹诺酮和磺胺类药物残留的同时检测.
Abstract
OBJECTIVE To establish a test method for the determination of residues of two quinolones enrofloxacin(ENR)and norfloxacin(NOR)and one sulfadiazine(SD)in milk by HPLC-MS in order to maintain the quality of milk.METHODS The aqueous phase was 0.1％formic acid aqueous solution and the organic phase was 0.1％formic acid acetonitrile.The mass spectrometry and chromatographic conditions were optimized and the quantification was performed by external standard method.RESULTS The concentrations of ENR,NOR and SD in the range of 10.00～l00.0ng·mL-1,10.00～150.00ng·mL-1 and 20.00～250.00ng·mL-1 were linear with R2 of 0.988,0.944 and 0.947.The recoveries were in the range of 90％～105％with the relative standard deviations(RSD,n=12)of 16％,9.4％and 9.6％at the spiked levels of ENR,NOR and SD of 25,100 and 1OOng·mL-1,and the limits of detection(LOD)of the method were 8.48,2.09 and 1.87ng·mL-1 and the limits of quantification(LOQ)were 9.94,9.78 and 15.35ng·mL-1.CONCLUSION The method has the advantages of high sensitivity and selectivity,and is suitable for the simultaneous determination of quinolone and sulfonamide residues in milk.
关键词
高效液相色谱串联质谱法/喹诺酮类药物/磺胺嘧啶/牛奶Key words
HPLC-MS/quinolones/sulfadiazine/milk引用本文复制引用
基金项目
国家级/省级陕西学前师范学院大学生创新创业训练计划(202114390023)
国家级/省级陕西学前师范学院大学生创新创业训练计划(S202114390023)
国家级/省级陕西学前师范学院大学生创新创业训练计划(2021DC23)
出版年
2024
NETL
NSTL
万方数据