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Objective To establish a rapid determination and analysis method for crotonoside, magnoflorine and isoguanine in food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 60% (volume fraction) acetonitrile aqueous solution. After vortex oscillation, ultrasonic extraction and high-speed centrifugation, the supernatant was filtered through a filter membrane and used for determination. The mobile phase consisted of acetonitrile-0.1% (volume fraction) formic acid aqueous solution for gradient elution. Separation was carried out on a Waters BEH Amide (3.0 mm×100 mm, 2.5 μm) chromatography column. The mass spectrometry was conducted using positive ion electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode for qualitative and quantitative determination of 3 kinds of alkaloids, namely crotonoside, magnoflorine and isoguanine. Results The linear relationship between 3 kinds of alkaloids was good within the corresponding mass concentration range (r>0.997), the average recoveries ranged from 83.7% to 102.3%, and the relative standard deviations were ranged from 3.2% to 7.4% (n=6). The limits of detection for crotonoside and magnoflorine were both 0.1 μg/L, and the limits of quantification were 1.0 μg/L. The limit of detection for isoguanine was 1.0 μg/L, and the limit of quantification was 2.0 μg/L. Conclusion This method has a rapid and simple sample pretreatment process, short time-consuming, high sensitivity and good accuracy, and is suitable for the rapid detection and confirmatory analysis of 3 kinds of alkaloids in emergency incidents of suspected croton poisoning.
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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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