超高效液相色谱-串联质谱法对动物源食品中13种林可胺类及大环内酯类药物残留的检测  

Determination of Lincosamides and Macrolides in Animal Origin Food by UPLC-MS/MS

作　　者：孙雷[1] 张骊[1] 王树槐[1] 汪霞[1] 

机构地区：[1]中国兽医药品监察所,北京100081

出　　处：《分析测试学报》2009年第9期1058-1061,1065,共5页Journal of Instrumental Analysis

基　　金：国家科技支撑计划课题资助项目(2006BAD31B09)

摘　　要：建立了动物源食品中林可霉素、克林霉素、吡利霉素、红霉素、泰乐菌素、螺旋霉素、替米考星、竹桃霉素、吉他霉素、克拉霉素、阿奇霉素、罗红霉素和交沙霉素13种林可胺类和大环内酯类药物残留检测的超高效液相色谱-串联质谱分析方法。动物组织样品经乙腈提取后,用正己烷去除脂肪等杂质,然后用Waters Acquity UPLC BEH C18色谱柱分离,以乙腈和50mmol/L乙酸铵水溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测模式检测。结果表明:13种药物在5～200μg/L范围内呈现良好的线性关系,相关系数R2均大于0.990,13种药物在动物组织中的检出限均为1μg/kg,定量下限均为2.5μg/kg。以2.5、25、100μg/kg3个水平进行回收实验,13种药物的回收率为72%～104%,批内批间相对标准偏差为4.8%～14.3%。A ultra performance liquid chromatography coulped to tandem mass spectrometry（ UPLC - MS/MS） method was established for the determination of lincomycin, clindymycin, pirlimycin, e- rythromycin, tylosin, spiramycin, timicosin, oleandomycin, kitasamycin, clarithromycin, azithro- mycin, roxithromycin, josamycin residue in animal origin food. Animal tissue samples were extrac- ted by acetonitrile, and the fat was removed by hexane. The separation of 13 lincosamides and mac- rolides was performed on Waters Acquity UPLC BEH C18 column by a gradient elution using acetoni- trile（A） -50 mmol/L ammonium acetate（B） as mobile phase with a flow rate of 0. 3 mL/min. The identification of 13 drugs were carried out by positive electrospray ionization （ESI＋ ） under multiple reaction monitoring（MRM） mode. The calibration curves were good linear between the peak areas and concentrations of 13 lincosamides and macrolides in the range of 5 -200 μg/L, with correlation coefficients more than 0. 990. The limits of detection and limits of quantification of 13 drugs in animal origin food were 1 Ixg/kg and 2.5 μg/kg, respectively. The average recoveries from spiked animal tissues at three concentration levels of 2. 5, 25 and 100 μg/kg ranged from 72% to 104%. The in- tra- and inter-RSDs were in the range of 4.8% - 14.3% .

关 键 词：超高效液相色谱-串联质谱 林可胺类 大环内酯类 残留 动物源食品 

分 类 号：O657.72[理学—分析化学] TQ460[理学—化学]