[Preparation of covalent organic framework based on room temperature solution-suspension approach and its application to solid-phase microextraction of pyrethroids in tea].

2021 
Pyrethroids (PYs) have been widely used to control pests and prevent diseases in tea gardens. However, with the increasingly stringent pesticide testing standards in the import and export trade of tea, there is an urgent need for methods to detect trace amounts of PYs in tea. In this study, a covalent organic framework (COF) material TpBD with excellent thermal/chemical stability, high porosity, and a large specific surface area was prepared by a room-temperature solution-suspension approach (SSA). TpBD-coated solid phase microextraction (SPME) fibers were fabricated by coating the material on etched stainless-steel fibers by a simple physical coating method. The fibers were used in combination with gas chromatography-tandem mass spectrometry (GC-MS/MS) to establish a highly sensitive method for the detection of PYs. The enrichment factors of this method for cyfluthrin, cypermethrin, flucythrinate, fenvalerate, and deltamethrin were 702-2687. The method showed low LODs (0.1-0.5 ng/L), wide linear ranges (0.2-800 ng/L), good linearities (correlation coefficients (R)≥0.9991) and acceptable repeatabilities (RSD≤11.0%, n=3). Green tea and oolong tea samples were analyzed using the developed method, and trace levels of the five PYs were successfully detected. The recoveries of the spiked PYs in the real green tea and oolong tea samples were in the range of 80.2%-109.5%. Experimental results showed that the established analytical method is suitable for the determination of PY pesticides in tea. Furthermore, the TpBD material was successfully prepared by the SSA method, demonstrating that the method has good universality and excellent potential for the simple synthesis of other COF materials.
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