| Objective To establish a method for detecting pentachlorophenol residues in various animal derived foods using ultra performance liquid chromatography-tandem mass spectrometry. Methods Triethylamine acetonitrile water extraction and mixed anion exchange column purification were used, and detected by ultra performance liquid chromatography-tandem mass spectrometer. This article had discussed in detail the key control points such as extraction, purification, nitrogen blowing, filtration, chromatographic-mass spectrometric separation, analysis, and qualitative and quantitative determination. The improved method optimized the proportion of extraction solvents and removed the nitrogen blowing and concentration process. Eventually, a determination method applicable to the residual amounts of pentachlorophenolic acid in muscles (pork, beef, mutton, chicken), livers (pig liver, beef liver, sheep liver, chicken liver), kidneys (pig kidney, beef kidney, sheep kidney, chicken kidney), fish, shrimp, crabs, shellfish, poultry eggs (chicken eggs, duck eggs, goose eggs, quail eggs), milk and milk powder was established. Results The pentachlorophenol were linear in the range of 0.2~8.0 ng/mL with correlation coefficients (r2) higher than 0.99. The limits of detection (S/N≥3) was 0.5 μg/kg, and the limits of quantification (S/N≥10) was 1.0 μg/kg. The recovery rates of different matrices at LOQ, 2LOQ, and 10LOQ spiked levels were all between 64.5% and 119.0%, with intra - and inter assay RSD less than 15%. Conclusion This method is simple, efficient, and accurate. It is suitable for the detection of pentachlorophenolic acid in different animal foods, which can provide technical support for regulating the behavior of drug use in breeding and ensuring the safety of animal food. |
