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Objective To study and screen the novel vardenafil derivative in food, and establish a quantitative method. Methods A compound with similar structure to vardenafil was detected in food by ultra performance liquid chromatography-quadrupole-exactive orbitrap-high resolution mass spectrometry. The molecular structure and fragmentation law of the vardenafil structure analogue were inferred from the fragment ions of high-resolution mass spectrometry. The compound name was clarity compared with the custom-synthesized reference substance. Quantitative analysis was carried out in a multiple reaction monitoring by high performance liquid chromatography-tandem triple quadrupole mass spectrometry with the external standard method. Results The novel vardenafil derivative in food was identified as propoxyphenyl hydroxy-vardenafil. The results showed that good linearity was observed for propoxyphenyl hydroxyvardenafil within the concentration range of 2-50 ng/mL. The limit of detection was 0.03 mg/kg, and the limit of quantitation was 0.10 mg/kg. The average recoveries and relative standard deviations (RSD) of coffee, confectionery, jelly and plant-based drinks were 87.6%-102.6% and 0.5%-6.3% respectively. The reproducibility and stability of the method were good (RSD<5%). The method was applied to measure the real samples, and 34 batches of positive samples were found with the content range of 1.60×103-2.62×104 mg/kg. -Conclusion This method is fast, accurate and high sensitivity, can be used for screening and quantitative determination of the derivative propoxyphenyl hydroxyvardenafil in food, and can provide technical support for the supervision of the illegal addition of vardenafil derivatives.
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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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