摘要
建立了含有C18填料的快速溶剂同步萃取净化结合超高效液相色谱-串联质谱同时测定养殖鱼肌肉中19种磺胺类药物残留的检测方法。基于快速溶剂萃取仪萃取,并在萃取池内同时加入样品、硅藻土和C18填料(吸附剂),以1%甲酸乙腈溶液进行同步萃取净化,提取液再经冷冻1 h去除杂质。经氮吹复溶后可直接采用ACQUITY UPLCTM BEH C18色谱柱分离,以0.1%甲酸水和乙腈作为流动相进行梯度洗脱。19种磺胺类药物残留在0.1~20.0 ng/mL范围内线性关系良好,相关系数均>0.990,方法检出限为0.1~0.5μg/kg。在5、10、15μg/kg加标浓度下,加标回收率为80.3%~108.6%,相对标准偏差为3.2%~10.5%。以该方法对多种水产鱼肌肉样品进行分析,共检出2种磺胺类药物残留。该方法简便、高效、灵敏度高、自动化程度高,适合大批量样品的准确定性和定量分析检测。
A method has been developed for simultaneous determination of 19 kinds of sulfonamides(SAs)residues in cultured fish muscle by using accelerated solvent extraction(ASE)and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).After the fish muscle was blended diatomite and C18,the mixture was packed into the extraction cell and the SAs were extracted with 1%formic acid acetonitrile.The extracts were evaporated to dryness,and redissolved with the initial mobile phase for UPLC-MS/MS analysis after freezing 1 h.The ectract was separated by a UPLCTM BEH C18 column,and gradiently eluted with 0.1%formic acid(A)and acetonitrile(B)as the mobile phase.The results showed that the recoveries were 80.3%~108.6%for 19 SAs at spiked levels of 5~15μg/kg,and the relative standard deviation(RSD)were 3.2%~10.5%.High correlation coefficients(R2>0.990)of 19 kinds of SAs within their linear ranges(0.1~20 ng/mL).The limit of detection(LOD)for the analytes was 0.1~0.5μg/kg.The method was applied to six samples buying in the market and 19 SAs were detected,in which SDZ and SMZ were detected.Using ASE the method was featured as short extraction times,high extraction yields,with high level of automation,and can meet the rapid and accurate detection requirements of sulfonamides residues in aquatic product.
作者
赵巧灵
张薇英
汤海凤
王萍亚
戴意飞
蒋玲波
ZHAO Qiaoling;ZHANG Weiying;TANG Haifeng;WANG Pingya;DAI Yifei;JIANG Lingbo(Zhoushan Institute for Food and Drug Control,Zhoushan 316000)
出处
《食品科技》
CAS
北大核心
2019年第12期335-341,共7页
Food Science and Technology
基金
舟山市公益类科技项目(2017C32077)
省分析测试科技计划项目(2017C37089).
关键词
快速溶剂萃取
超高效液相串联质谱
磺胺类药物残留
养殖鱼
accelerated solvent extraction(ASE)
utra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
sulfonamides residues
cultured fish
作者简介
赵巧灵(1985—),女,浙江舟山人,博士,工程师,研究方向为色谱分析检测;通信作者:张薇英
