Full
Outline
To establish a method for the determination of 12 kinds of antiviral drugs (ATVs) in shellfish and dried shellfish products by ultra performance liquid chromatography-tandem mass spectrometry.
Samples were extracted with acetonitrile containing 1% formic acid, purified using FaVEx-NM50 multi-veterinary drug residue clean-up columns, concentrated under nitrogen in a water bath, and reconstituted with a redissolving solution to obtain the test solution. The analytes were separated on a ZORBAX Eclipse Plus C18 column using gradient elution with a mobile phase consisting of acetonitrile‑methanol (80:20, V:V, containing 0.1% formic acid) and 5 mmol/L ammonium acetate (containing 0.1% formic acid). Detection was carried out by ultra performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode, and quantification was performed using the internal standard method.
The 12 kinds of target compounds showed good linearity over certain concentration ranges, and the limits of detection and recoveries met the requirements. The correlation coefficients (r) of the calibration curves ranged from 0.9931 to 0.9997, limits of detection were 0.07–1.50 μg/kg, and limits of quantitation were 0.14–3.00 μg/kg. At 3 spiked levels (n=6), the average recoveries in mussel matrix ranged from 66.7% to 106.2% with relative standard deviations of 1.0%–11.6%,while in dried scallop matrix the average recoveries ranged from 69.1% to 109.5% with relative standard deviations of 0.9%–10.3%. Meanwhile, 161 batches of shellfish and dried shellfish products were purchased and analyzed for the target compounds using this method. The results showed that amantadine was detected in 37 batches. A dietary exposure risk assessment of amantadine residues was conducted by combining the residue data with dietary consumption and population data. The assessment indicated that the current amantadine residues in shellfish posed a low risk to human health.
The method is sensitive, accurate, simple and rapid in sample pretreatment,making it suitable for the determination of ATVs residues in shellfish.
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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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