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Objective To establish a method for the determination of pentachlorophenol residues in various animal derived foods by 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) were 0.3 µg/kg, and the limits of quantitation (S/N≥10) were 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 relative standard deviation (RSD) less than 15%. Conclusion The method is simple to operate, highly accurate, and has good applicability, which can meet the detection of pentachlorophenol residues in different animal derived foods.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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