摘要
建立了快速测定鳗鱼中氯霉素药物残留的超高效液相色谱串联三重四极杆质谱（UPLC—MS／MS）分析方法。样品添加同位素内标后，经1％HCl水解，乙酸乙脂提取、净化、流动相溶解，通过Waters ACQUITY UPLC^TM BEH C18色谱柱分离，以串联质谱在多反应监测（MRM）模式下测定，在2min内完成氯霉素的定量分析。结果表明：氯霉素在0．02—1．0μg／kg浓度范围内线性良好，相关系数（r）为0．9965；在0．05、0．1、0．5μg／kg添加水平条件下，氯霉素加标回收率为86．6％-92．5％，相对标准偏差（RSD）均小于7％（n=5）；本方法对氯霉素检出限和定量限分别为0．003μg／kg和0．011μg／kg。
An ultra performance liquid chromatography -tandem mass spectrometry （UPLC -MS/MS） method was developed to determine the residue of chloramphenicol in eel. The samples, labled by the isotopicaUy internal standard, were finally dissolved in the mobile phase after the procedure of hydrolysis by 1% HCl, extraction by ethyl acetate, and purification. Chromatographic separation was achieved by using a Waters ACQUITY UPLC^TM BEH C18 column and the detection was performed by tandem mass spectrometry under the mode of multiple reaction monitoring （MRM）. The quantitative analysis of chloramphenicol was finished within 2 min. Results showed that in the range of 0.02 - 1.0 μg/kg the standard curves for chloramphenicol were in good linearity, and the correlation coefficients （r） was 0. 996 5. The recoveries for chloramphenicol at the addition of three levels （0. 05, 0. 1, 0. 5 μg/kg） were ranged from 86. 6% to 92.5% and the relative standard deviation （RSD） for the determination of chloramphenicol was less than 8% （n = 5）. The limit of quantity （LOQ） and limit of determination （LOD） by the present method for chloramphenicol were found to be 0. 003 μg/kg and 0.011 μg/kg respectively.
出处
《中国兽药杂志》
2007年第11期20-23,共4页
Chinese Journal of Veterinary Drug
关键词
超高效液相色谱-串联质谱法
氯霉素
鳗鱼
ultra performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）
chloramphenicol
eel
