QuEChERS-超高效液相色谱-串联质谱法测定鱼和虾中苯巴比妥残留  

Determination of phenobarbital residues in fish and shrimp by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：黄佳佳[1] 杨慧晴 温惠敏 邓龙[1] 杨昭[1] 李燕杰[1] 丘婷婷 徐振林[3] HUANG Jia-Jia;YANG Hui-Qing;WEN Hui-Min;DENG Long;YANG ZhaoLI Yan-Jie;QIU Ting-Ting;XU Zhen-Lin(College of Food Science,Guangdong Food and Drug Vocational College,Guangzhou 510520,China;Guangdong Test Center for Green Labelling Co.,Ltd.,Guangzhou 510440,China;College of Food Science,South China Agricultural University,Guangzhou 510642,China)

机构地区：[1]广东食品药品职业学院食品学院,广州510520 [2]广东省绿色产品认证检测中心有限公司,广州510440 [3]华南农业大学食品学院,广州510642

出　　处：《食品安全质量检测学报》2022年第12期3794-3802,共9页Journal of Food Safety and Quality

基　　金：国家自然科学基金项目(32061160473);广东省普通高校重点研究项目(2019KJDXM002);广东省普通高校青年创新人才类项目(2019GKQNCX063);广东省食品检测创新团队项目(2021KCXTD077);广东食品药品职业学院食品营养与检测教学创新团队项目(2020TD02);广东食品药品职业学院科研项目(2017ZR024)。

摘　　要：目的建立QuEChERS样品前处理结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定鱼和虾中苯巴比妥残留的方法。方法样品采用乙腈提取,经乙二胺-N-丙基硅烷(primary secondary amine,PSA)、C18、石墨化碳黑(graphitized carbon black,GCB)和无水硫酸镁(MgSO4)净化,使用Agilent Eclipse Plus C18色谱柱(50 mm×2.1mm,1.8µm)分离,以甲醇(A)-水(B)为流动相进行梯度洗脱,在UPLC-MS/MS多反应监测模式下进行定性和定量分析。结果方法在0.5~100.0μg/L的质量浓度范围内线性关系良好,相关系数(r 2)为0.9999,检出限和定量限分别是0.5、1.5µg/kg。草鱼、鲈鱼、罗非鱼和南美白对虾4种常见鲜活水产品经QuEChERS前处理,有效降低基质干扰,表现为可忽略的弱基质效应。对以上4种样品进行加标回收实验,平均回收率为72.1%~96.7%,相对标准偏差为1.2%~12.3%(n=6)。结论该方法操作简便快速、灵敏度高、准确性和精密度好,可满足水产品鱼和虾中苯巴比妥残留快速筛查和定量分析的需求。Objective To develop a method for the determination of phenobarbital residues in fish and shrimp by pre-treatment of QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted by acetonitrile solution,purified with primary secondary amine(PSA),C18,graphitized carbon black(GCB),anhydrous magnesium sulfate(MgSO4),and separated by Agilent Eclipse Plus C18 column(50 mm×2.1 mm,1.8μm)by gradient elution using methanol(A)-water(B)as mobile phase.The qualitative and quantitative analyses were carried out under the multiple reaction monitoring modes of UPLC-MS/MS.Results This method had good linear relationship in the range of 0.5‒100.0μg/L,and the correlation coefficient(r 2)was 0.9999.The limits of detection and quantitation were 0.5 and 1.5µg/kg,respectively.Four kinds of common fresh aquatic products including Ctenopharyngodon idellus,Lateolabrax japonicus,Oreochroms mossambcus and Litopenaeus Vannamei pre-treated with QuEChERS could effectively reduce matrix interference,showing a negligible weak matrix effect.The average recoveries of the above 4 kinds of samples were 72.1%‒96.7%,and the relative standard deviations were 1.2%‒12.3%(n=6).Conclusion The proposed method is simple,fast,sensitive,accurate and precise,which is suitable for rapid and quantitative analysis of phenobarbital residues in fish and shrimp samples.

关 键 词：苯巴比妥 鱼 虾 QUECHERS 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]