Full
Outline
To establish a method for screening illegally added sedative-hypnotic compounds in functional foods by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry.
Samples were extracted with acetonitrile or 1% ammonia-acetonitrile (by volume fraction), purified with 50 mg N-propylethylenediamine and 150 mg anhydrous magnesium sulfate, and separated using a Waters BEH C18 column (2.1 mm×100 mm, 1.7 μm). The mass spectrometry analysis was performed in positive and negative ion switching scan mode, combined with full-scan primary mass spectrometry and data-dependent tandem mass spectrometry acquisition. Based on the established multilevel database of sedative-hypnotic compounds, high-throughput qualitative screenings and analysis of the target compounds were achieved.
All sedative-hypnotic compounds showed good linear relationships in the concentration range of 10–600 µg/kg, with correlation coefficients all greater than 0.99, and the limits of quantitation ranged from 20 to 50 µg/kg. In compressed candies, liquid beverages and mixed milk powders, the average spiked recoveries (mass fraction) were 51.03%–119.92%, 53.36%–115.46% and 51.89%–116.79%, respectively; the relative standard deviations were 1.19%–9.75%, 1.27%–9.93% and 1.24%–9.52%, respectively. In the screening of actual samples, the detection rate of melatonin was 22%.
The proposed method is simple to operate, highly sensitive, and it is applicable for determining illegally added sedative-hypnotic compounds in diverse food matrices, providing robust technical support for food safety 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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