摘要
建立动物源食品中同时检测4种青霉素类药物残留的高效液相色谱法。以水合氨苄青霉素为内标,样品经乙腈-水(10:1,V/V)提取,HLB固相萃取小柱净化。采用C_(18)色谱柱,以0.02 mol/L磷酸二氢钾溶液-乙腈为流动相,梯度洗脱分离目标化合物进行定量分析。青霉素G、苯唑西林、乙氧萘青霉素、双氯青霉素在0.01~2μg/mL范围内线性良好,线性相关系数均大于0.999,检出限和定量限分别为3μg/kg和10μg/kg;回收率在69.9%~100.3%之间,精密度的相对标准偏差在1.58%~9.15%之间。该方法前处理简单、快速、准确、灵敏,可以满足实际检测分析的需要。用于猪、牛、羊、鸡、鱼等不同基质中青霉素类药物残留的检测,取得了满意的结果。
A high performance liquid chromatography(HPLC)method for the determination of four penicillin residues in foods of animal origin was developed.Ampicillin trihydrate was used as the internal standard.Samples were extracted with a mixture of acetonitrile and water(10:1,V/V),and the extract was then cleaned up on an HLB solid-phase extraction cartridge.Penicillin G,oxacillin,nafcillin and dicloxacillin were separated on a C18column by gradient elution with a mobile phase consisting of monopotassium phosphate(0.02mol/L)and acetonitrile.The calibration curves were linear over the concentration range of0.01–2μg/mL with correlation coefficients of more than0.999.The limits of detection(RSN>3)(LOD)and quantification(RSN>10)(LOQ)were3and10μg/kg for all the analytes,respectively.The average recoveries were between69.9%and100.3%with relative standard deviations(RSDs)of1.58%–9.15%(n=6).The method is simple,rapid,sensitive and accurate and can meet the requirements for practical analysis.It has been applied with satisfactory results to detect penicillin residues in pork,beef,chicken and fish.
作者
马燕红
王妍
李志刚
李莹莹
郭文萍
MA Yanhong;WANG Yan;LI Zhigang;LI Yingying;GUO Wenping(China Meat Research Center, Beijing 100068, China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2018年第24期317-321,共5页
Food Science
基金
北京市优秀人才培养资助项目(2016754154700G147)
关键词
青霉素类
动物源性食品
高效液相色谱法
penicillin
animal origin foods
high performance liquid chromatography
作者简介
第一作者:马燕红(1984—),女,高级工程师,博士,主要从事肉制品检测及香味分析研究。E-mail:jcmyh@126.com.