QuEChERS净化结合高效液相色谱串联质谱法快速测定果蔬中四唑虫酰胺残留  

Determination of tetraniliprole residue in fruits and vegetables by QuEChERS purification combined with HPLC-MS/MS

作　　者：邓航 朱礼 张可欣 袁列江 李政 吴海智 上官佳 陈瑶 薛敏敏 王秀 李格 孙逸清 DENG Hang;ZHU Li;ZHANG Kexin;YUAN Liejiang;LI Zheng;WU Haizhi;SHANGGUAN Jia;CHEN Yao;XUE Minmin;WANG Xiu;LI Ge;SUN Yiqing(Hunan Provincial Institute of Product and Goods Quality Inspection,Changsha 410007,China;Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410111,China;Yueyang Inspection and Testing Center,Yueyang 410042,Hunan,China)

机构地区：[1]湖南省产商品质量检验研究院,长沙410007 [2]食品安全监测与预警湖南省重点实验室,长沙410111 [3]岳阳市检验检测中心,湖南岳阳410042

出　　处：《农药》2024年第12期904-910,924,共8页Agrochemicals

基　　金：湖南省自然科学基金科技项目(2022JJ90032)。

摘　　要：[目的]建立了一种Qu ECh ERS净化结合高效液相色谱串联质谱法快速测定果蔬中四唑虫酰胺残留的分析方法。[方法]样品经乙腈提取,Qu ECh ERS净化包(含无水硫酸钠4 g,无水硫酸镁4 g,PSA 200 mg,C_(18)100 mg)净化,在Agilent Venusil MP C_(18)上分离,以甲醇和水为流动相进行梯度洗脱,采用电喷雾离子化,负离子扫描,多反应监测模式(SRM)进行检测,用基质匹配外标法定量。[结果]四唑虫酰胺在不同果蔬基质下0.1~20μg/L线性范围内相关系数(r)均大于0.999。方法检出限(S/N≥3)为0.10μg/kg,定量限(S/N≥10)为0.50μg/kg。以金针菇、胡萝卜、韭菜、四季豆、包菜、白菜、番茄、黄瓜、桃子、南非脐橙、葡萄、火龙果、西瓜为基质,四唑虫酰胺在0.50、1.00、5.00μg/kg3个水平加标回收率在82.86%~99.15%之间,相对标准偏差(RSD,n=6)在0.10%~6.79%之间。[结论]方法操作方便、处理快速、具备高准确性和灵敏度,可满足果蔬中四唑虫酰胺残留的检测工作要求。[Aims]The present study aims to establish a rapid analytical method for the determination of tetraniliprole residues in fruits and vegetables using QuEChERS purification combined with HPLC-MS/MS.[Methods]The samples were extracted with acetonitrile and purified using a QuEChERS purification package which consisted of anhydrous sodium sulfate(4 g),anhydrous magnesium sulfate(4 g),PSA(200 mg)and C_(18)(100 mg).Separation was achieved on Agilent Venusil MP C_(18) column with gradient elution of methanol and water as the mobile phase.Detection was performed by electrospray ionization in negative ion scanning mode using multi-reaction monitoring(SRM)technique,while quantification was carried out through matrix matching external standard method.[Results]The correlation coefficients(r)of tetraniliprole within the linear range of 0.1-20μg/L across various matrices consistently exceeded 0.999.The method exhibited a detection limit(S/N≥3)of 0.10μg/kg and a limit of quantification(S/N≥10)of 0.50μg/kg.Spiked recoveries at levels of 0.50,1.00 and 5.00μg/kg in various matrices including Flammulina velutipe,carrot,leek,kidney bean,cabbage,tomato,cucumber,peach,rock candy orange,grape,pitaya and watermelon ranged from 82.86%to 99.15%with relative standard deviations(RSD,n=6)ranging from 0.10%to 6.79%.[Conclusions]The method is convenient,fast,and highly accurate and sensitive,fully meeting the requirements for detecting tetraniliprole residues in fruits and vegetables.

关 键 词：高效液相色谱质谱/质谱联用仪 QUECHERS 四唑虫酰胺 残留 

分 类 号：TQ450.2[化学工程—农药化工]