液相色谱-电喷雾串联质谱法检测鸡组织中5种聚醚类药物残留  

Determination of 5 polyether antibiotics in chicken tissues by liquid chromatography-electrospray ionization tandem mass spectrometry

作　　者：梁春来[1] 程林丽[1] 沈建忠[1] 张玉洁[1] 张素霞[1] 

机构地区：[1]中国农业大学动物医学院,国家兽药残留基准实验室,北京100193

出　　处：《色谱》2009年第6期815-819,共5页Chinese Journal of Chromatography

基　　金：“十一五”国家科技支撑计划项目(No.2006BAK02A08-3)

摘　　要：建立了鸡组织中聚醚类药物多残留检测的高效液相色谱-电喷雾串联质谱方法。采用甲醇提取鸡组织中的拉沙洛菌素、盐霉素、莫能菌素、甲基盐霉素和马杜霉素,经硅胶柱净化,以乙腈(含0.1%甲酸)-0.1%甲酸水溶液(体积比为97∶3)为流动相,Symmetry Shield RP18作为色谱分析柱,多反应监测(MRM)正离子扫描方式进行质谱检测。当5种聚醚类药物的添加水平为鸡肉0.1～1 500μg/kg、鸡肝0.2～4 500μg/kg时,平均回收率为71.6%～99.1%,日内测定的相对标准偏差(RSD)(n=5)为3.2%～10.7%,日间RSD(n=3)为4.6%～14.7%。2种鸡组织中5种聚醚类药物的定量限为0.1～1.0μg/kg。该方法的灵敏度、准确度和精密度均符合兽药残留分析技术的要求,适用于鸡肉和鸡肝中5种聚醚类药物的多残留检测。A liquid chromatography-electrospray ionization tandem mass spectrometry （LC-ESI MS/MS） method for the determination of 5 polyether antibiotics （ lasalocid, salinomycin, monensin, narasin and maduramicin ） in chicken tissues was developed. The polyether antibiotics were extracted from chicken tissues with methanol. The extract was evaporated to dry, and redissolved in hexane, then cleaned up on a Sep-Pak Silica solid-phase extraction cartridge. The target drugs were eluted with 6 mL methylene chloride-methanol （90： 10, v/v）, and the eluate was collected and dried under a gentle stream of nitrogen gas, then the residue was dissolved with l mL acetonitrile （ containing 0. 1% formic acid） and analyzed by LC-MS/MS. The LC sep- aration was performed on a Symmetry Shield reversed phase C18 bonded silica column with acetonitrile （ containing 0. 1% formic acid） - 0. 1% formic acid （ 97： 3, v/v） as mobile phase. The quantification was carried out by positive electrospray ionization and multiple reaction monitoring （ MRM ） mode. The validation was carried out on spiked chicken muscle （ spiked at 0. 1 - 1 500 μg/kg） and chicken liver （ spiked at 0.2 - 4 500μg/kg）, the average recoveries of target drugs ranged from 71.5% -99. 1% with intra-day relative standard deviations （RSDs） of 3.2% - 10.7% and inter-day RSDs of 4.5% - 14.7%. The limits of quantification （LOQs） in chicken muscle and liver were 0. 1 - 1.0 μg/kg. The results demonstrated that the sensitivity, accuracy and precision of this method meet the requirements of veterinary drug residue analysis. The method is applicable to detect 5 polyether antibiotics in chicken muscle and liver.

关 键 词：液相色谱-电喷雾串联质谱法 聚醚类药物 鸡肉 鸡肝 

分 类 号：O658[理学—分析化学]