Wang Xiao-Li, Geng Hong-Shuai, Liu Lu, Zhao Ling-Xi, Li Na, Jiang Hai-Long, Wang Xia, Chen Xiang-Feng, Zhao Ru-Song
Qilu University of Technology (Shandong Academy of Sciences), Shandong Analysis and Test Center, Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Jinan 250014, China.
J Agric Food Chem. 2025 Apr 23;73(16):9994-10002. doi: 10.1021/acs.jafc.4c10843. Epub 2025 Apr 13.
Establishing an effective method for insecticide residue analysis is critical for food safety control. This study reported a convenient and sensitive approach for extracting and analyzing trace chloronicotinyl insecticides (CNIs) in honey samples. A magnetic covalent organic framework (FeO@PyTTA-DHPA-COFs) was synthesized and employed as an adsorbent in magnetic solid phase extraction (m-SPE). The FeO@PyTTA-DHPA-COFs exhibited efficient and rapid adsorption (5 min) for CNIs. The m-SPE-HPLC-MS/MS method for trace analysis of CNIs in honey samples was established with good linearity (0.5-200 ng g) and a low limit of quantitation (0.05-0.95 ng g). CNI residues (0.93-4.38 ng g) were detected in real honey samples, much lower than the maximum residue levels (MRLs) of CNIs in honey. The recoveries of CNIs in spiked honey samples were 72.1-106% with RSD < 9.5%. The successful application demonstrates the potential of this method in trace analysis of CNIs residues.
建立一种有效的杀虫剂残留分析方法对于食品安全控制至关重要。本研究报道了一种简便、灵敏的方法，用于提取和分析蜂蜜样品中的痕量氯代烟碱类杀虫剂（CNIs）。合成了一种磁性共价有机框架（FeO@PyTTA-DHPA-COFs），并将其用作磁性固相萃取（m-SPE）中的吸附剂。FeO@PyTTA-DHPA-COFs对CNIs表现出高效、快速的吸附（5分钟）。建立了用于蜂蜜样品中CNIs痕量分析的m-SPE-HPLC-MS/MS方法，线性良好（0.5-200 ng/g），定量下限低（0.05-0.95 ng/g）。在实际蜂蜜样品中检测到CNI残留量为（0.93-4.38 ng/g），远低于蜂蜜中CNIs的最大残留限量（MRLs）。加标蜂蜜样品中CNIs的回收率为72.1-106%，相对标准偏差<9.5%。该方法的成功应用证明了其在CNIs残留痕量分析中的潜力。
