液相色谱-质谱联用法测定水产品中头孢菌素类残留量  

Study on Determination of Cephalosporins in Aquatic Products by Liquid Chromatography Tandem Mass Spectrometry

作　　者：顾蓓乔[1] 梅光明[1] 喻亮[1] 张小军[1] 朱敬萍[1] 李佩佩[1] 

机构地区：[1]浙江海洋学院海洋与渔业研究所,浙江省海洋水产研究所,浙江舟山316021

出　　处：《浙江海洋学院学报（自然科学版）》2015年第3期222-226,共5页Journal of Zhejiang Ocean University(Natural Science Edition)

基　　金：浙江省科技计划项目(2012F20026)

摘　　要：建立了水产品中3种头孢菌素类药物残留的液相色谱-串联质谱检测方法。样品用乙腈提取、正己烷脱脂净化后,经减压浓缩、流动相定容后用0.22μm微孔滤膜过滤,用超高效液相色谱-三重四级杆质谱仪(UPLC-MS/MS)进行检测,外标法定量。头孢噻呋、头孢氨苄和头孢喹肟的定量检出限分别为2.00μg/kg,2.00μg/kg和10.0μg/kg;3种头孢菌素标准溶液在2~100μg/L质量浓度范围内均呈良好的线性关系(r^2均大于0.995);在10~100μg/kg加标范围内,头孢氨苄平均回收率范围为76.7%~93.1%,头孢喹肟平均回收率范围为80.5%~93.9%,头孢噻呋平均回收率为78.9%~87.2%,批内相对标准偏差均小于13%。研究结果表明该方法回收率高、精密度好,可满足水产品中头孢菌素类药物残留量的检测要求。A ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method was developed for determination of 3 cephalosporins. Samples were extracted with acetonitrile and further defatted by n-hexane liquid-liquid extraction, and then the solvent was vaporized and analytes were dissolved with mobile phase. After filtrated through 0.22 μm membrane UPLC-MS/MS was used for detection, with external standard method as the quantitative method. Quantitative limits of Ceftiofur, Cephalexin and Cefquinome were 2.00 μg/kg, 2.00 μg/kg and 10.0 μg/kg, respectively. In the concentration range of 2-100 μg/L, 3cephalosporins showed good linear relationship（r^2 all above 0.995）. Spiked at levels of 10-100 μg/kg, the average recovery rates were 76.7.2%-93.1%,80.5%-93.9% and 78.9%-87.2% for Cephalexin, Cefquinome and Ceftiofur. The relative standard deviations were less than 13%. The results show that this method can be suc-cessfully applied for the determination of cephalosporins drug residue in aquatic products with good reproducibility and high recovery.

关 键 词：液相色谱-质谱联用法 水产品 头孢菌素 

分 类 号：R927.1[医药卫生—药学]