动物源性食品中激素类、喹诺酮类、氯霉素类兽药残留同时检测方法研究  

Simultaneous Determination of Hormone,Quinolone and Chloramphenicol Veterinary Drug Residues in Food of Animal

作　　者：刘楚楚 贺丽苹[1,3] Liu Chuchu;He Liping(South China Agricultural University,Guangzhou 510642;Guangdong Food and Cosmetics Testing Center,Guangzhou 510670;Instrumental Analysis&Research Center,South China Agricultural University,Guangzhou 510642,China)

机构地区：[1]华南农业大学,广东广州510642 [2]广东省保化检测中心有限公司,广东广州510670 [3]华南农业大学测试中心,广东广州510642

出　　处：《广东化工》2022年第21期199-202,共4页Guangdong Chemical Industry

摘　　要：本研究运用高效液相色谱-串联质谱法(HPLC-MS/MS),结合固相萃取(SPE)前处理技术,建立动物源性食品中激素类、喹诺酮类、氯霉素类71种兽药残留同时检测方法。样品采用0.1%甲酸-0.1%乙酸乙腈溶液进行提取,以4%氯化钠沉淀蛋白质,正己烷进行脱脂,HLB固相萃取柱净化;五氟代苯基(PFP)色谱柱进行分离,以0.1%甲酸水溶液、0.1%乙酸-乙腈溶液为流动相,进行梯度洗脱,MRM模式测定。结果显示,激素类、喹诺酮类、氯霉素类三类共71种组分在2~300 ng/mL浓度范围内,相关系数r均大于0.99,线性关系良好,方法检出限在0.01~1μg/kg,方法回收率为80%~120%,相对标准偏差为1.1%~8.9%。本方法准确度和精密度良好,适用于动物源性食品中激素类、喹诺酮类、氯霉素类药物残留大批量样品快速检测。In this study,high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)combined with solid phase extraction(SPE)pretreatment technique was used to establish a method for simultaneous determination of 71 veterinary drug residues in animal food.The sample was extracted with 0.1%formic acid-0.1%acetic acid acetonitrile solution,protein was precipitated with 4%sodium chloride,defatted with n-hexane,and purified by HLB solid phase extraction column.Pentafluorophenyl(PFP)column was used for separation.0.1%formic acid aqueous solution and 0.1%acetic acid-acetonitrile solution were used as mobile phase for gradient elution and MRM mode determination.The results showed that 71 components of hormones,quinolones and chloramphenicol were in the range of 2~300 ng/mL concentration,the correlation coefficients were all more than 0.99,and the linear relationship was good.The detection limit of the method was 0.01~1μg/kg,the recovery rate was 80%~120%,and the relative standard deviation was 1.1%~8.9%.The method has good accuracy and precision and is suitable for rapid detection of hormone,quinolone and chloramphenicol residues in animal food.

关 键 词：动物源性食品 激素类 喹诺酮类 氯霉素类 高效液相色谱-串联质谱法 固相萃取法 

分 类 号：TS201.6[轻工技术与工程—食品科学]