Objective To establish a method for the simultaneous determination of 16 kinds of anesthetics and metabolites residual amount in aquatic products by multi-plug filtration cleanup (m-PFC)-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Samples were extracted with acetonitrile containing 1% formic acid, separated by salting-out, and the upper acetonitrile was purified by m-PFC column packed with anhydrous magnesium sulfate, primary secondary amine (PSA), and enhanced matrix removal-lipid (EMR-Lipid). The targets were separated by C18 column using methanol-2 mmol/L ammonium formate containing 0.1% formic acid as mobile phase for gradient elution, detected by positive or negative electrospray ionization-tandem mass spectrometry under multiple reaction monitoring mode, and quantified with matrix external standard method. Results The 16 kinds of anesthetcs and metabolites showed good linear relationships in their respective concentration ranges (r2>0.996). The limits of detection (S/N=3) and limits of quantitation (S/N=10) were 0.03-0.30 μg/kg and 0.10-1.00 μg/kg. The average recoveries at low, medium and high concentration levels in the blank sample matrix were 79.3%-113.8%, and the relative standard deviations were 1.3%-7.2% (n=6). Conclusion This method is simple to operate, sensitive and good in stability, which can be applied to the rapid detection of 16 kinds of anesthetics and metabolites in aquatic products.
| 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 |