Xia Xi, Li Xiaowei, Ding Shuangyang, Shen Jianzhong
China Agricultural University, College of Veterinary Medicine, Department of Pharmacology and Toxicology, Beijing 100193, People's Republic of China.
J AOAC Int. 2010 Sep-Oct;93(5):1666-71.
A sensitive and reliable method has been developed and validated for the determination of chloramphenicol in poultry and swine liver using SPE and ultra-performance liquid chromatography (UPLC)/MS/MS. The liver samples were extracted with ethyl acetate, defatted with n-hexane, and further cleaned up using SPE cartridges with polymeric sorbent. An Acquity BEH C18 column was used for gradient UPLC separation, with water and acetonitrile as the mobile phase. The multiple reaction monitoring mode was used for two precursor-product ion transitions for chloramphenicol and one for the internal standard. The method was validated at 0.1, 0.3, and 1.0 microg/kg. Mean recoveries from fortified samples ranged from 95.5 to 106.7% with an RSD of 12.2%. The method LOD was < 0.02 microg/kg.
已开发并验证了一种灵敏且可靠的方法，用于使用固相萃取（SPE）和超高效液相色谱（UPLC）/串联质谱（MS/MS）测定家禽和猪肝中的氯霉素。肝脏样品用乙酸乙酯萃取，用正己烷脱脂，然后使用带有聚合物吸附剂的SPE柱进一步净化。使用Acquity BEH C18柱进行梯度UPLC分离，以水和乙腈作为流动相。采用多反应监测模式对氯霉素的两个前体-产物离子跃迁和内标的一个跃迁进行监测。该方法在0.1、0.3和1.0微克/千克水平进行了验证。加标样品的平均回收率为95.5%至106.7%，相对标准偏差为12.2%。该方法的检测限<0.02微克/千克。
