Simultaneous Determination of 19 Kinds of Chlorophenols in Fish Samples by Ultra-Performance Liquid Chromatography- Quadrupole-Time of Flight-Mass Spectrometry

A method for simultaneous determination of 19 kinds of chlorophenols (CPs) in fish samples by ultra -performance liquid chromatography-quadrupole-time of flight-mass spectrometry (UPLC-Q-TOF-MS) was developed. The samples were pretreated using QuEChERS method. Exactly, the sample was ultrasonic extracted by ethyl acetate, and the supernatant was concentrated to near dry by blowing nitrogen after purification by C18 and MgSO4. Finally, the UPLC-Q-TOF-MS in the negative ion scanning mode using atmospheric pressure chemical ionization source was used for on-machine detection. ACQUITY UPLC BEH C18 column (100 mm x 2.1 mm, 1.7 & mu;m) was used as the chromatographic column, and the mixture of acetonitrile-1 mmol/L ammonium formate at the flow rate of 0.4 mIlmin was used as the mobile phase. The column and sample temperature were 30 and 20 & DEG;C, respectively. The acquisition mode was MS scan, and the detection spectrum library of 19 kinds of CPs was also established. The results showed that the linearity of this method was good in the range of 10-1500 & mu;g/L (R2 & GE;. 0.991). The limits of detection of 19 kinds of CPs were 5-10 & mu;g/kg, the limits of quantitation were 16-30 & mu;g/kg, and the recoveries were 65.7%-98.2% with the relative standard deviations of less than 10%. The matrix effects of 19 kinds of CPs ranged from 0.64 to 2.24. The method developed here was of great theoretical and practical significance for control and management of residual level of phenolic compounds in aquatic products.