Efficient Solid-Phase Extraction of Neonicotinoid Insecticides from Environmental Water and Drink Samples Using a...

Neonicotinoid insecticides (NNIs) are extensively utilized globally because of their efficient and broad-spectrum properties. However, their residues are also extensively distributed in the environment. Herein, MIL-101-SO₃Na with abundant -NH- and sulfonate groups was synthesized via chloromethylation and nucleophilic substitution postmodification strategies and used to extract NNIs via solid-phase extraction. MIL-101-SO₃Na was enhanced by introducing C-H···N hydrogen bonds to strengthen interaction forces and -SO₃Na groups to adjust surface charge and enhance electrostatic attraction. This modification and the substantial specific surface area (998 m²·g^-1) of the metal-organic framework markedly enhanced the enrichment efficiency of MIL-101. The proposed method based on MIL-101-SO₃Na exhibited a minimal detection threshold (0.04-0.87 ng·L^-1), an extensive linear spectrum (1-2000 ng·L^-1), and notable accuracy (a variation of 3.02-11.8%) in water and drink samples. NNI concentrations between 0.25 and 24.2 ng·L^-1 in fruit juice and tea samples were accurately identified using the proposed method, demonstrating its feasibility in practical applications. The postmodification of MIL-101-SO₃Na is an exceptional and promising approach for the sensitive detection of ultratrace NNI levels in complex matrices.