液相色谱串联质谱法测定猪肉和牛肉中双氯酚酸、氟尼辛、加米霉素的残留量  

Determination of Diclofenac,Flunixin and Gamithromycin in Pork and Beef by HPLC-MS/MS

作　　者：烟利亚[1] YAN Li-ya(Shanghai Intertek Testing Services Co.,Ltd.,Shanghai 200233,China)

机构地区：[1]上海天祥质量技术服务有限公司,上海200233

出　　处：《广州化工》2024年第13期82-86,共5页GuangZhou Chemical Industry

摘　　要：建立了采用液相色谱串联质谱仪(HPLC-MS/MS)同时检测猪肉和牛肉中双氯芬酸、氟尼辛、加米霉素残留量的分析方法。样品用乙腈提取,氮吹近干后,乙腈水(1+1)复溶,过膜后采用LC-MS/MS分析,电喷雾离子源正模式扫描,外标法定量。双氯芬酸、加米霉素的线性范围为5~100 ng/mL;氟尼辛的线性范围为0.5~10 ng/mL;线性相关系数均大于0.99。双氯芬酸、加米霉素的方法检出限为1μg/kg,氟尼辛的方法检出限为0.1μg/kg。低、中、高3水平添加回收率在60%~120%之间,精密度均小于10%。该方法检出限低、准确度高、操作简便,可以高效处理批量样品。An analytical method for the simultaneous detection of diclofenac,flunixin and gamithromycin residues in pork and beef by liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was established.The samples were extracted with acetonitrile,dried by nitrogen blowing,reconstituted in acetonitrile water(1+1),analyzed by LC-MS/MS after passing through the membrane,scanned in positive mode by electrospray ion source,and quantified by external standard method.The linear ranges of diclofenac and gamithromycin were 5~100 ng/mL.The linear range of flunixin was 0.5~10 ng/mL.The linear correlation coefficients were all greater than 0.99.The limit of detection of diclofenac and gamithromycin were 1μg/kg,and that of flunixin was 0.1μg/kg.The recovery rate of low,medium and high levels were between 60%~120%,and the precisions were less than 10%.This method has a low detection limit,high accuracy,and easy operation,and can efficiently process batch samples.

关 键 词：液相色谱串联质谱法 双氯芬酸 氟尼辛 加米霉素 

分 类 号：O657.72[理学—分析化学]