摘要
目的建立固相萃取-超高效液相色谱-串联质谱法检测牛奶中喹诺酮类抗生素残留。方法牛奶样品用0.2%甲酸乙腈溶液超声提取,上清液经PRiME HLB小柱净化后液氮气吹至近干,用5%甲醇水溶液复溶,最后注入LC-MS/MS检测分析,采用Waters ACQUITY UPLCTMBEH C18柱为分析柱,基质匹配外标法定量。结果 9种喹诺酮类药物在0.50~20.0μg/L具有良好的线性关系,相关系数r=0.999 1~0.999 9,加标回收率为96.1%~131%,相对标准偏差小于20%,方法检出限为0.031 5~0.422μg/kg,方法定量限为0.105~1.41μg/kg。结论该方法简便快速,灵敏可靠,适用于牛奶中喹诺酮类抗生素残留的批量测定。
Objective To determine 9 quinolones residues in milk by using a method based on solid phase extraction and ultra performance liquid chromatography coupled with tandem mass spectrometry(LC-MS/MS). Method The milk sample was ultrasonic extracted with 0.2% formic acid-acetonitrile and purified by PRiME HLB column. Then, the eluent was collected and dried under nitrogen,further dissolved with 5% methanol water and determined by LC-MS/MS. Waters ACQUITY UPLCTMBEH C18 column was used for separate,and the matrix-matching external standard method was used to quantify. Results 9 quinolone antibiotics showed good linearities within range of 0.50-20.0 μg/L,and the correlation coefficients(r)were0.999 1-0.999 9. The average recovery rates of9 quinolone antibiotics were 96.1%-131%, and the relative standard deviation(RSD) were less than 20%. The detection and quantitation limits of this method were 0.031 5-0.422 μg/kg and 0.105-1.41 μg/kg, respectively. Conclusion This method is simple, rapid, sensitive and reliable, and is suitable for the rapid determination of quinolone antibiotics residues in milk.
作者
雍莉
江阳
王艳
崔淑丹
徐先顺
胡彬
邹晓莉
YONG Li;JIANG Yang;WANG Yan;CUI Shudan;XU Xianshun;HU Bin;ZOU Xiaoli(Centre for Disease Prevention and Control of Sichuan Province,Chengdu 610041,Sichuan Province,China;West China School of Public Health,Sichuan University,Chengdu 610041,Sichuan Province,China)
出处
《预防医学情报杂志》
CAS
2020年第9期1196-1200,共5页
Journal of Preventive Medicine Information
