超高效液相色谱-串联质谱法检测婴幼儿辅助食品中多种兽药残留  

Determination of multi-veterinary drug residues in complementary foods for infants and young children by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：罗瑞涟 吴正双 梁炽琼 罗丽婷 LUO Ruilian;WU Zhengshuang;LIANG Chiqiong;LUO Liting(Foshan Center for Food and Drug Control,Foshan 528051,China;The 5th People’s Hospital of Foshan City,Foshan 528200,China)

机构地区：[1]佛山市食品药品检验检测中心,广东佛山528051 [2]佛山市第五人民医院,广东佛山528200

出　　处：《色谱》2022年第12期1076-1086,共11页Chinese Journal of Chromatography

摘　　要：生产婴幼儿辅助食品的原辅料中常常含有鱼类、肉类、肝类等动物性组织,存在兽药残留的风险,为了更加全面地对这类产品进行安全监管,研究并开发了同时检测婴幼儿辅助食品中6大类(喹诺酮类、磺胺类、大环内酯类、硝基咪唑类、氯霉素类和抗病毒类)50种抗生素和抗病毒类兽药残留的超高效液相色谱-三重四极杆质谱法(UPLC-MS/MS)。样品采用酸化乙腈超声提取,提取液经新型的脂质增强型Captiva EMR-Lipid固相萃取柱净化,浓缩复溶后采用流动相乙腈和0.1%(v/v)甲酸水溶液,经C18柱梯度洗脱分离,电喷雾多反应监测(MRM)模式检测,基质匹配外标法定量。结果显示,该方法50种兽药在0.5~50μg/L范围内线性关系较好,相关系数均不低于0.995,方法检出限为0.03~0.70μg/kg,定量限为0.09~2.33μg/kg。50种化合物在不同基质中,添加5和50μg/kg两个加标水平进行试验,平均回收率为64.37%~119.3%,相对标准偏差均小于15%。将该方法应用于14份国产和6份进口的婴幼儿辅助食品检测,结果显示,1份进口肉类婴幼儿辅助食品中检出磺胺喹噁啉、磺胺二甲嘧啶和替米考星。该方法简单快速,灵敏度和准确度高,样品量消耗少,适用于婴幼儿辅助食品中多种兽药残留的检测。Special attention must be paid to children and infants because health issues stemming from a poor immunologic system and low weight make them a vulnerable risk group.Complementary foods for infants and young children,which are a class of special dietary foods,are essential transitional foods for infants from lactation to adaptation to ordinary food.Some complementary foods for infants and young children are of animal origin such as fish,meat,and the liver,which may contain veterinary drug residues.Veterinary drugs are usually small-molecular-weight chemicals that are essential for treating infections,increasing production,and improving animal husbandry.However,abuse of these substances can provoke transfer to the food chain,leading to negative consequences for humans,especially infants and young children.For a more comprehensive safety supervision of infant supplementary foods,a method based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed and used for the determination of 50 antibiotics and antivirals(grouped into six categories:fluoroquinolones,sulfonamides,macrolides,nitroimidazoles,chloramphenicols,and antivirals)in complementary foods for infants and young children.The matrix of complementary foods for infants and young children is complex and contains a large number of proteins and lipids,which poses a serious challenge for sample pretreatment.The Captiva EMR-Lipid solid-phase extraction(SPE)column is a new type of product that allows for selective and efficient lipid/matrix removal without negatively affecting the recovery of the analyte.In this study,samples were extracted with acidified acetonitrile and then purified using a Captiva EMR-Lipid SPE column.The target analytes were separated on a BEH C18 column by gradient elution using acetonitrile and water containing 0.1%(v/v)formic acid as the mobile phases.MS detection was performed with an electrospray source in the positive and negative modes in the multireaction monitoring(MRM)mode.The ion spray voltages we

关 键 词：固相萃取净化 超高效液相色谱-串联质谱 多兽药残留 婴幼儿辅助食品 

分 类 号：O658[理学—分析化学]