基于分子印迹固相萃取/LC-MS/MS联用技术检测渔业环境中甲霜灵及其代谢物残留OA
Determination of Metalaxyl and Its Metabolite Residues in Aquaculture Environments Using Molecularly Imprinted Solid-phase Extraction Combined with LC-MS/MS
以(噁)霜灵为虚拟模板,甲基丙烯酸与丙烯酰胺为二元功能单体,乙二醇二甲基丙烯酸酯为交联剂,偶氮二异丁腈为引发剂,采用沉淀聚合法合成了一种对甲霜灵具有选择性吸附功能的分子印迹聚合物.通过扫描电子显微镜和傅里叶变换红外光谱对聚合物的形貌和结构进行了表征,并结合等温吸附实验及吸附动力学实验研究了其选择性识别机制.结果表明,该印迹材料对甲霜灵及其代谢物甲霜灵酸具备高吸附容量和强特异性识别能力.将所制备的聚合物填充为固相萃取小柱,结合液相色谱-串联质谱(LC-MS/MS)技术,建立了渔业环境中甲霜灵及甲霜灵酸的检测方法.该方法在1~200 ng/mL范围内线性良好,r²>0.997.目标分析物在水体和底泥中的检出限分别为1.25、2.34 ng/L和0.15、0.29 ng/g,定量下限(LOQ)分别为4.16、4.81 ng/L和0.38、0.60 ng/g,加标回收率为86.1%~105%,相对标准偏差(RSD)不大于8.2%.该方法操作简便、灵敏度高、抗干扰能力强,适用于渔业环境中上述痕量目标物的日常监测.
This study synthesized a molecularly imprinted polymer(MIP)selective for metalaxyl us-ing oxadixyl as a dummy template,methacrylic acid and acrylamide as binary functional monomers,ethylene glycol dimethacrylate as a cross-linker,and azodiisobutyronitrile as an initiator via precipi-tation polymerization.The polymer was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy,and its adsorption behavior was evaluated through isothermal and ki-netic experiments.Results confirmed high affinity and specificity toward metalaxyl and its metabolite,metalaxyl acid.The MIP was employed as a solid-phase extraction sorbent coupled with liquid chro-matography-tandem mass spectrometry(LC-MS/MS)for the analysis of aquaculture water and sedi-ment samples.The method demonstrated good linearity(r²>0.997)from 1 to 200 ng/mL,with aver-age recoveries of 86.1%-105%and relative standard deviations not more than 8.2%.Detection limits were 1.25,2.34 ng/L in water and 0.15,0.29 ng/g in sediment,and quantification limits were 4.16,4.81 ng/L in water and 0.38,0.60 ng/g in sediment,respectively.This method is sensitive,robust,and straightforward,which is suitable for routine monitoring of trace metalaxyl residues in aquaculture environments,supporting sustainable aquaculture practices.
李佳豪;周豪;尹怡;林嘉薇;赵城;单奇;王庆
福建农林大学 海洋学院,福建 福州 350002||中国水产科学研究院珠江水产研究所,广东 广州 510380中国水产科学研究院珠江水产研究所,广东 广州 510380中国水产科学研究院珠江水产研究所,广东 广州 510380中国水产科学研究院珠江水产研究所,广东 广州 510380中国水产科学研究院珠江水产研究所,广东 广州 510380中国水产科学研究院珠江水产研究所,广东 广州 510380福建农林大学 海洋学院,福建 福州 350002||中国水产科学研究院珠江水产研究所,广东 广州 510380
化学化工
甲霜灵甲霜灵酸分子印迹固相萃取液相色谱-串联质谱渔业环境
metalaxylmetalaxyl acidmolecularly imprinted solid-phase extractionLC-MS/MSaquaculture environments
《分析测试学报》 2026 (3)
543-550,8
国家自然科学基金(32503192,32303012)广州市科技计划项目(2023A04J0091)中国水产科学研究院中央级公益性科研院所基本科研业务费(2023TD49)
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