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Objective To establish a method for the determination of malachite green, crystal violet, leucomalachite green and leuco crystal violet in fish by solid-phase extraction (SPE) combine with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was subjected to protein precipitation and extraction with acetonitrile, followed by pass-through purification using an HMR-Lipid SPE column. The analytes were then separated by the BEH shield C18 chromatographic column using a mobile phase gradient with acetonitrile and ammonium acetate. The positive ion mode of the electrospray ionization source was used for multiple reaction monitoring (MRM) scanning, and the internal standard method was used for quantification. Results The linear ranges of the 4 kinds of target analytes were 0.20-10.00 ng/mL, with correlation coefficient (r) more than 0.999. The limit of detection was 0.05 μg/kg. The recoveries at 3 spiking levels (2, 5, 10 μg/kg) were 80.1%-105.2%, and the relative standard deviations were 1.2%-14.3%. Conclusion The method is rapid, sensitive and accurate, and is suitable for the determination of malachite green, crystal violet and their leuco metabolites in fish. It can provide support for quality control and market supervision.
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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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