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Outline
To establish a method for determination the 4 kinds of androgen residues, namely testosterone, methyltestosterone, trenbolone and 17 β-trenbolone acetate in pork by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry.
The pork samples were homogenized after comminution. Subsequently, water and acetonitrile solution were added sequentially for extraction by oscillation.Anhydrous magnesium sulfate and sodium chloride were introduced for dehydration, followed by centrifugation. The supernatant was collected and purified by adsorption using anhydrous magnesium sulfate and neutral alumina.The purified solution was dried under nitrogen in a water bath at 45 ℃, then redissolved by vortexing in an acetonitrile-water mixture (1:1, V:V). After filtration through a 0.22 μm microporous membrane, the solution was ready for analysis. For the determination of analytes, an ACQUITY UPLC BEH C18 column (2.1 mm×100 mm,1.7 μm) was adopted. Acetonitrile and 0.1% formic acid aqueous solution were used as the mobile phase for chromatographic separation. Data acquisition was performed in the electrospray ionization positive mode with multiple reaction monitoring, and quantification was carried out via the external standard method.
The target compounds exhibited good linearity in the concentration range of 0.1–100.0 ng/mL, with all correlation coefficients (r2) greater than 0.999. The limits of detection were 0.1–0.3 μg/kg, and the limits of quantitation were 0.2–1.0 μg/kg. At the spiking levels of 2, 8 and 20 μg/kg, the recoveries were between 84.12% and 109.75%, with the relative standard deviations varying from 1.72% to 9.62%.
This method can simultaneously determine 4 kinds of androgens and the pretreatment is simple. It has high sensitivity, repeatability and accuracy and can provide a reference for related detection.
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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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