高效液相色谱串联质谱检测奶粉中喹诺酮类药物残留量  

Determination of Quinolone Residues in Milk Powder by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：王军锋 李安 闫璐璐 张慧君 庞兴萍 曹文玉 WANG Junfeng;LI An;YAN Lulu;ZHANG Huijun;PANG Xingping;CAO Wenyu(School of Chemistry&Chemistry Engineering,Shaanxi Xueqian Normal University,Xi'an 710100;Qingdao Experimental High School,Qingdao 266109)

机构地区：[1]陕西学前师范学院化学化工学院,西安710100 [2]山东省青岛市实验高级中学,青岛266109

出　　处：《食品工业》2022年第6期319-323,共5页The Food Industry

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(项目编号:202114390023,S202114390023,2021DC23)。

摘　　要：采用高效液相色谱串联质谱(high performance liquid chromatography tandem mass spectrometry,HPLC-MS)法建立3种喹诺酮药物(恩诺沙星、环丙沙星、诺氟沙星)残留量的检测方法。试验优化色谱和质谱的条件、样品前处理及以外标法定量的分析过程。结果表明,在2.50~50.00 ng/mL区间内具有良好的线性关系,恩诺沙星、环丙沙星、诺氟沙星的相关系数分别为0.998,0.999和0.996。在加标量5 ng条件下,3种化合物的加标回收率为83.5%~90.2%,相对标准偏差(SRSD,n=12)为7.8%~14%,检出限为0.35~0.82 ng/mL,定量限为0.37~0.92 ng/mL。高效液相色谱串联质谱法快速、高效并且准确,能够同时检测多种喹诺酮类药物。使用该方法检测出的奶粉结果精准,并且符合兽药残留检测标准,具有良好的应用前景。High performance liquid chromatography tandem mass spectrometry(HPLC-MS)was used to establish a method for the detection of three typical quinolone drugs(enrofloxacin,ciprofloxacin,norfloxacin).The experiment was carried out to optimize the condition of chromatography and mass spectrometry,sample pretreatment,and quantitative analysis process with external standard method.The results showed that there was a good linear relationship in the interval of 2.50-50.00 ng/m L,and the correlation coefficients of enrofloxacin,ciprofloxacin,and norfloxacin were 0.998,0.999,and 0.996,respectively.When the spiked amount was 5 ng,the spiked recoveries of the three compounds were between 83.5%and 90.2%;The relative standard deviation(SRSD,n=12)was between 7.8%and 14%,and the detection limit was between 0.35 ng/mL and 0.82 ng/mL;The limit of quantification was between 0.37 ng/mL and 0.92 ng/mL.High performance liquid chromatography tandem mass spectrometry was rapid,efficient and accurate,and could detect a variety of quinolones at the same time.The result of milk powder detected by this method was accurate,and meets the detection standard of veterinary drug residues,which had a good application prospect.

关 键 词：高效液相色谱串联质谱 喹诺酮药物 奶粉 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]