Yu Qidong, Zhang Lan, Zhang Wenmin, Yang Jiangfan
College of Horticulture, Fujian Agriculture and Forestry University, Fuzhou 350002, China.
Ministry ofEducation Key Laboratory of Analytical Science of Food Safety and Biology, Fuzhou University, Fuzhou 350116,China.
Se Pu. 2021 Apr 8;39(4):349-356. doi: 10.3724/SP.J.1123.2020.12012.
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 ()≥0.9991) and acceptable repeatabilities (RSD≤11.0%, =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.
拟除虫菊酯(PYs)已被广泛用于茶园害虫防治和疾病预防。然而,随着茶叶进出口贸易中农药检测标准日益严格,迫切需要检测茶叶中痕量PYs的方法。本研究采用室温溶液悬浮法(SSA)制备了具有优异热/化学稳定性、高孔隙率和大比表面积的共价有机框架(COF)材料TpBD。通过简单的物理涂覆方法将该材料涂覆在蚀刻不锈钢纤维上,制备了TpBD涂层固相微萃取(SPME)纤维。将这些纤维与气相色谱-串联质谱(GC-MS/MS)联用,建立了一种高灵敏度检测PYs的方法。该方法对氯氟氰菊酯、氯氰菊酯、氟氰戊菊酯、氰戊菊酯和溴氰菊酯的富集因子为702 - 2687。该方法具有低检测限(0.1 - 0.5 ng/L)、宽线性范围(0.2 - 800 ng/L)、良好的线性关系(相关系数()≥0.9991)和可接受的重复性(RSD≤11.0%,=3)。使用所建立的方法对绿茶和乌龙茶样品进行分析,成功检测到了痕量的5种PYs。在实际绿茶和乌龙茶样品中加标PYs的回收率在80.2% - 109.5%范围内。实验结果表明,所建立方法适用于茶叶中PY类农药的测定。此外,通过SSA法成功制备了TpBD材料,表明该方法具有良好的通用性以及简单合成其他COF材料的巨大潜力。