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Objective To Establish a method for simultaneous determination of 11 kinds of caine anesthetics and their 3 kinds of metabolites in aquatic products by QuEChERS-liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by acetonitrile, dehydrated by anhydrous MgSO4 and NaCl, purified by 100 mg primary secondary amine (PSA), filtered by 0.22 µm organic microporous membrane, and qualitatively and quantitatively determined by liquid chromatography-tandem mass spectrometry. Results The 11 kinds of caine anesthetes and their 3 kinds of metabolites showed a good linear relationship in the mass concentration range of 0.01-5.00 μg/L, and the correlation coefficients (r) were 0.99529-0.99989. The limit of detection (LOD) and the limit of quantification (LOQ) of 11 kinds of caine anesthetics and their 3 kinds of metabolites were 0.05-2.00 µg/kg and 0.15-5.00 µg/kg, respectively. The 3 kinds of substrates, white shrimp, carp and turbinus were performed at 3 levels: 1 times LOQ, 2-2.5 times LOQ and 10 times LOQ. The recoveries of 11 kinds of caine anesthetics and their 3 kinds of metabolites in 3 samples were 71.3%-114.2%, 71.2%-107.0% and 70.4%-104.5%, and the relative standard deviations were 0.7%-11.2%, 0.5%-11.5% and 0.8%-14.2%. The method was used to detect 50 batches of different varieties of aquatic products in the market. The results showed that 4 batches of products were detected with caine anesthetic, and the other 46 batches were not detected, the detection rate was 8%. The detected items were mainly tricaine, benzocaine, m-aminobenzoic acid and p-aminobenzoic acid, the content of which were 5.68-90.80 μg/kg, and the other 10 kinds of compounds were not detected. Conclusions The method is simple and fast, has high sensitivity, accuracy and precision, and can simultaneously determine a variety of caine anesthetics in aquatic products. It is suitable for the determination of batch samples, and has high practical application significance, and can provide powerful technical support for food safety monitoring.
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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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