高效液相色谱-串联质谱法测定动物肌肉组织中氯霉素、甲砜霉素和氟苯尼考残留量

采用液相色谱-串联质谱(LC-MS/MS)法测定动物肌肉组织中氯霉素,甲砜霉素和氟苯尼考三种药物的残留量。添加氘代氯霉素(d5-氯霉素)作为内标,碱化乙酸乙酯提取,正己烷去除脂肪,省去固相萃取步骤直接上机定量。选择电喷雾离子源(ESI),负离子扫描多反应监测(MRM)模式,并优化了质谱参数,使仪器的灵敏度达到最高。氯霉素、甲砜霉素和氟苯尼考的检出限均达到0.01μg/kg。空白样品中添加氯霉素、甲砜霉素和氟苯尼考水平为0.02～1μg/kg时,三种药品的线性相关系数均大于0.9990。氯霉素平均回收率为92.8%～97.0%,甲砜霉素平均回收率为93.5%～96.6%,氟苯尼考平均回收率为91.2%～95.9%。

High Performance Liquid Chromatography-Tandem Mass Spectrometric Determination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Animal Muscles

A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the determination of chloramphenicol,thiamphenicol and florfenicol in animal muscles.Samples were spiked with deuterated chloramphenicol-d5(d5-CAP) as internal standard and extracted with alkaline ethyl acetate.The resulting extract was then treated with n-hexane for the removal of lipids and injected directly into the HPLC-MS/MS system without the requirement of solid-phase extraction clean-up.The electr...