Objective To establish a method for the determination of 17α-estradiol and 17β-estradiol in aquatic products by QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with water-acetonitrile (2:8, V:V), purified with N-propylethylenediamine, C18 and neutral alumina, blown to dryness with nitrogen, and then reconstituted with water-acetonitrile (8:2, V:V). The sample solution was analyzed using water and acetonitrile (both containing 5 mmol/L ammonia) as mobile phase, separated by C18 chromatographic column, scanned and detected in multiple reaction monitoring (MRM) mode, and quantified by external standard method. Results The results showed that 17α-estradiol and 17β-estradiol showed a good linear relationship in the concentration ranges of 5 to 200 μg/L, and the correlation coefficients were 0.9998 and 0.9985, respectively. The average recoveries at three spiked concentration levels varied from 66.5% to 101.1% with relative standard deviations of 0.62% to 10.17%. The limit of detection was 0.85-0.90 μg/kg, and the limit of quantitation was 2.1-2.4 μg/kg. Conclusion This method is simple, fast, sensitive and accurate, suitable for qualitative and quantitative analysis of 17α-estradiol and 17β-estradiol in aquatic products such as fish, shrimp, crabs and shellfish.
| 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 |