多壁碳纳米管改进QuEChERS净化结合高效液相色谱串联质谱法快速测定水产品中四唑虫酰胺残留  

Multi-walled carbon nanotubes improved QuEChERS extraction combined with HPLC-MS/MS for rapid determination of tetraniliprole residues in aquatic products

作　　者：袁列江 张可欣 李政 朱礼 邓航 吴海智 陈瑶 薛敏敏 上官佳 王秀 李格 孙逸清 YUAN Liejiang;ZHANG Kexin;LI Zheng;ZHU Li;DENG Hang;WU Haizhi;CHEN Yao;XUE Minmin;SHANGGUAN Jia;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,China)

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

出　　处：《食品与发酵工业》2025年第3期349-358,共10页Food and Fermentation Industries

基　　金：湖南省自然科学基金科技项目(2022JJ90032)。

摘　　要：该文建立了一种多壁碳纳米管(multi-walled carbon nanotube,MWCNTs)改进QuEChERS净化结合高效液相色谱串联质谱法快速测定水产品四唑虫酰胺残留的分析方法。样品经乙腈提取,无水硫酸钠4 g,无水硫酸镁4 g分离水相和有机相,MWCNTs改进QuEChERS(每毫升提取液加入3 mg MWCNTs,60 mg C18,50 mg PSA)净化包净化,在Agilent Venusil MP C18(100 mm×2.1 mm,3μm)上分离,以甲醇和水为流动相,电喷雾离子化,负离子扫描,多反应监测模式检测,基质匹配外标法定量。结果显示,四唑虫酰胺在不同水产品基质下0.1~20μg/L线性范围内相关系数(R^(2))均大于0.999。方法定量限(S/N≥10)为0.80μg/kg。以草鱼、带鱼、小龙虾、基围虾、大闸蟹、梭子蟹、花甲为基质,四唑虫酰胺在2.0、4.0、20μg/kg 3个水平加标回收率为82%~97%,批内相对标准偏差(relative standard deviation,RSD,n=6)为0.66%~4.02%,批间RSD(n=6)为0.88%~2.95%。本方法便捷高效,可满足水产品中四唑虫酰胺残留的检测工作要求。An analytical approach was developed for the rapid determination of tetraniliprole hydrochloride residues in aquatic products.This method involved a modified QuEChERS extraction combined with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)and multi-walled carbon nanotubes(MWCNTs).The samples were extracted using acetonitrile,and then partitioned into aqueous and organic phases by adding 4 g of anhydrous sodium sulfate and 4 g of anhydrous magnesium sulfate.The purification process involved the use of MWCNTs-improved QuEChERS,which included the addition of 3 mg of MWCNTs,60 mg of C18,and 50 mg of PSA to each milliliter of extraction solution.Subsequently,the samples were separated on Agilent Venusil MP C18(100 mm×2.1 mm,3μm)column,eluted with a methanol-water mixture,ionized via electrospray ionization in negative ion mode,and quantified using multiple reaction monitoring(MRM)with matrix matching external standard calibration.The results showed that the relationship coefficient(R^(2))of tetraniliprole in different aquatic product matrices at 0.1-20μg/L was greater than 0.999.The quantitative limit of method(S/N≥10)was 0.80μg/kg.The recovery rates at 2.0μg/kg,4.0μg/kg,and 20μg/kg for carp,yellowtail,crayfish,grass shrimp,hairy crab,swimming crab,and clam as matrix were between 82% and 97% with relative standard deviation(RSD)of 0.66%-4.02%(n=6)for intra-batch and RSD of 0.88%-2.95%(n=6)for inter-batch.The method is convenient and efficient,and can meet the requirements for the detection of tetraniliprole residues in aquatic products.

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

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]