快速滤过型净化结合液相色谱-质谱联用法测定茶叶中特丁硫磷及其5种代谢产物

建立快速滤过型净化(multi-plug filtration cleanup,m-PFC)结合三重四极杆液相色谱-质谱联用技术同时检测茶叶中特丁硫磷及其5种代谢产物的方法.茶叶样品加水浸润后经过乙腈提取,盐析分层,取上层提取液经m-PFC柱净化,三重四极杆液相色谱-质谱联用仪测定,基质外标法定量.结果表明在1～500...

Determination of Terbufos and Its Five Metabolites in Tea By Multi-Plug Filtration Cleanup Method Combined with Liquid Chromatography-Tandem Mass Spectrometry

A method for simultaneous detection of terbufos and its five metabolites in tea by multi-plug filtration cleanup (m-PFC) method combined with liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was established. The pesticides in tea samples were extracted with acetonitrile after being fully wetted with water. Inorganic salts were added to the system to separate it into organic and aqueous phases. The upper fraction was purified on an m-PFC column before analysis by LC-MS/MS. The accurate quantification was performed by the matrix-matched external standard method. The results showed that the calibration curves for six pesticides (terbufos, terbufos sulfoxide, terbufos sulfone, terbufos-OXON, terbufos-OXON sulfoxide, and terbufos-OXON sulfone) had good linearity in the concentration range of 1–500 μg/L with correlation coefficients higher than 0.999. The detection limits were in the range of 0.001–0.01 mg/kg, and the quantitation limits were 0.002–0.03 mg/kg. The average recoveries at three spiked levels of 0.01, 0.50 and 2.00 mg/kg were in the range of 81.5%–103.9%, with relative standard deviations (RSDs) of 0.9%–10.1%. This method has the advantage of low cost and easy operation, and rapid analysis with good recovery and accuracy, and is suitable for simultaneous determination of the residues of terbufos and its metabolites in tea.