液质联用法测定牛奶中氯霉素类药物残留  

Determination of Chloramphenicols Residues in Milk by LC-MS/MS

作　　者：王浩[1] 杨红梅[1] 郭启雷[1] 

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《食品研究与开发》2015年第6期74-76,共3页Food Research and Development

基　　金：国家质检总局科技计划项目(2013QK332)

摘　　要：建立了牛奶中氯霉素、甲砜霉素和氟甲砜霉素多残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经碱性乙腈超声提取,以MGⅢ-C18色谱柱(2.1×150 mm,5μm)分离,流动相为10 mmol/L乙酸铵水溶液和甲醇(梯度洗脱),流速0.25 m L/min。采用多反应监测负离子模式,可以同时对牛奶中的氯霉素、甲砜霉素和氟甲砜霉素进行定性和定量测定。方法的检出限为0.1μg/kg^0.3μg/kg。在0.3、3.0、10.0μg/kg 3个加标水平下,加标回收率为80.7%~93.6%,相对标准偏差为3.85%~9.35%。A quick confirmative method was developed for determining the residues of chloramphenicol , thiamphenicol and florfenicol in milk by LC-MS/MS. The sample was ultrasonic extracted with alkaline acetonitrile, the HPLC separation was carried out on a MGⅢ-C18 column （2.1×150 mm, 5μm）,the mobile phase were 10 mmol/L ammonium acetate solution and methanol with gradient elution , the flow was 0.25 mL/min.The detection of chloramphenicol , thiamphenicol and florfenicol were carried out in the negative multi-reaction monitoring （MRM）mode. Under the optimal conditions, good linear relationship were obtained in the range of 0.1 μg/kg-50.0 μg/kg for chloramphenicol , thiamphenicol and florfenicol.The limit of detection were in the range of 0.1μg/kg-0.3μg/kg. The recoveries at three spiked levels of 0.3、3.0、10.0μg/kg were between 80.7%and 93.6%, and RSDs value were between 3.85%and 9.35%.

关 键 词：液质联用仪 牛奶 氯霉素类药物 残留 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]