高效液相色谱-串联质谱法同时测定鸡肉中氯霉素类药物及其代谢物残留方法的建立  

Development of method for simultaneous determination of chloramphenicol,thiamphenicol,florfenicol and florfenicol amine residues in chicken tissues by LC-MS/MS

作　　者：张伟玮[1] 曾明华[1] 许世富[2] 汤春莲[2] 杨娜[1] 欧俊秀[1] 王中宝[1] 吴丽君[1] 

机构地区：[1]安徽农业大学动物科技学院,合肥230036 [2]安徽省兽药饲料监察所,合肥230095

出　　处：《安徽农业大学学报》2012年第4期641-645,共5页Journal of Anhui Agricultural University

摘　　要：建立了鸡肌肉中氯霉素、甲砜霉素、氟苯尼考及氟苯尼考胺残留检测的液相色谱-串联质谱(LC-MS/MS)分析方法。样品在碱性条件下用乙酸乙酯提取后,再用正己烷去除脂肪,MCX小柱净化,洗脱液经浓缩,0.22μm滤膜过滤后,用高效液相色谱-串联质谱测定。采用电喷雾电离正负离子切换,多反应监测(MRM)模式测定。4种药物在2～100 ng·mL-1的系列浓度范围内均呈良好线性关系,相关系数r均大于0.990。样品中氯霉素的检测限为0.1μg.kg-1,定量限为0.3μg.kg-1;氟苯尼考的检测限为0.2μg.kg-1,定量限为0.5μg.kg-1;甲砜霉素和氟苯尼考胺的检测限为1.0μg.kg-1,定量限为3.0μg.kg-1。4种药物在0.2～2.0μg.kg-1的添加浓度范围内,平均回收率为79.3%～97.3%,相对标准偏差(RSD)均小于20%。满足了鸡肉中氯霉素、甲砜霉素和氟苯尼考残留的确证分析,同时对其主要代谢产物氟苯尼考胺进行了痕量监测。A liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was developed for the simultaneous determination of chloramphenicol（CAP）, thiamphenicol（TAP）, florfenicol （FF） and florfenicol amine（FFA） in chicken tissues. The samples were extracted by ethyl acetate in basic conditions, defatted with hexane and evaporated to dryness, followed by a clean-up step using the solid phase extraction with MCX. The eluent was filtered through 0.22μtm membrane and then analyzed by LC-MS/MS. Mass spectral acquisition was done using electrospray ionization in the switched ion mode applying multiple reaction monitoring. The calibration curve of mixed standard solution showed a good linearity in the concentration range from 2 to 100 ng.mL^-11 with the correla- tion coefficients（r） more than 0.990. The LOD （ limit of detection） of chloramphenicol was 0.1 μg.kg, and the limit ofquantification（LOQ） was 0.3 μg.kg-1. The LOD of florfenicol was 0.2μg.kg-1, and the LOQ was 0.5 μg.kg Both the LODs of thiamphenicol and florfenicol amine were 0.2 μg.kg-1, and the LOQs were 1.0μg.kg-1. The average re- coveries of 4 drugs ranged from 79.3% to 97.3%. The relative standard deviation （RSD） of the method was less than 20%. The method is useful for monitoring chloramphenicol, thiamphenicol and florfenicol residues in chicken tissues, and the most important metabolite can also be separated and quantitated.

关 键 词：氯霉素 甲砜霉素 氟苯尼考 氟苯尼考胺 液相色谱-串联质谱法 鸡 残留 

分 类 号：S852.23[农业科学—基础兽医学]