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

作　　者：王军锋 李安 庞兴萍 曹文玉 闫璐璐 WANG Jun-feng;LI An;PANG Xing-ping;CAO Wen-yu;YAN Lu-lu(School of Chemistry&Chemistry Engineering,Shaanxi Xueqian Normal University,Xi′an 710100,China)

机构地区：[1]陕西学前师范学院化学化工学院,陕西西安710100

出　　处：《化学工程师》2024年第8期22-26,共5页Chemical Engineer

基　　金：国家级/省级陕西学前师范学院大学生创新创业训练计划项目资助(202114390023,S202114390023,2021DC23)。

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,R^(2)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。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 10.00~100.0ng·mL^(-1),10.00~150.00ng·mL^(-1)and 20.00~250.00ng·mL^(-1)were linear with R~2 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 100ng·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)were9.94,9.78 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 

分 类 号：TS252.2[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]