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Outline
To establish an isotope dilution high performance liquid chromatography-tandem mass spectrometry method for the quantitative analysis of N-phenylpropoxyphenyl carbodenafil in health foods.
The samples were ultrasonically extracted with methanol, and the extracts were centrifuged, filtered and then analyzed. Chromatographic separation was performed on a RP18 column (2.1 mm×100 mm, 1.7 μm) used gradient elution with 2 mmol/L ammonium formate aqueous solution and acetonitrile as the mobile phase. Detection was carried out using electrospray ionization in positive ion mode with multiple reaction monitoring, and quantification was achieved using an isotope internal standard method.
N-phenylpropoxyphenyl carbodenafil showed good linearity in the range of 0.1–40.0 ng/mL, with a correlation coefficient greater than 0.995. The limit of detection was 0.005 mg/kg, and the limit of quantitation was 0.010 mg/kg. The recoveries at low, medium and high spiked levels ranged from 83.99% to 110.25%, with relative standard deviation (RSD) ranging from 3.1% to 13.1%. This method was applied to analyze 28 batches of collected samples, and none of them tested positive for N-phenylpropoxyphenyl carbodenafil.
This method is efficient, sensitive and accurate, effectively correcting matrix-induced ionization suppression in complex matrices, and is suitable for the qualitative and quantitative analysis of illegally added N-phenylpropoxyphenyl carbodenafil in health 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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