Full
Outline
To establish a method for the determination of 19 kinds of sex hormone residues in Pheretima by QuEChERS combined with enhanced matrix removal-lipid (EMR-lipid) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
The samples were pretreated using a QuEChERS dispersive solid-phase extraction combined with an EMR-lipid solid-phase extraction cleanup method.Separation was achieved on a Zorbax Eclipse Plus C18 column (3.0 mm×150 mm, 1.8 μm) using a gradient elution with a mobile phase consisting of 0.02% ammonia solution and methanol. Detection was performed by multiple reaction monitoring (MRM) in positive and negative electrospray ionization modes.
The 19 kinds of analytes were showed good linearity within their respective concentration ranges, with correlation coefficients all above 0.999. The average recoveries at 3 spiked levels ranged from 71.39% to 118.78%, with relative standard deviations ranging from 0.90% to 14.33%. The limits of detection were 2.5 μg/kg to 25.0 μg/kg, and the limits of quantitation were 5.0 μg/kg to 50.0 μg/kg.
This method exhibits high specificity and accurate results. It is suitable for the complex matrix of lipid-rich traditional Chinese medicines such as Pheretima and has been successfully applied to the detection of practical samples.
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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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