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To establish a screening method for the detection of adulteration of Draconis Sanguis in Zhenghonghua oil.
To establish a thin layer chromatography (TLC) method with 7, 4’-dihydroxyflavone as an index for fast screen of the adulteration in Zhenghonghua oil. The suspected samples were screened by TLC and the quantification was performed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The chromatographic column was SuperLu C18 (2)(100 mm×2.1 mm, 1.8 μm), the mobile phase was acetonitrile-water (25∶75) at a flow rate of 0.3 mL·min-1 and the column temperature was 25 ℃. The detection ion pairs for 7, 4’-dihydroxyflavone were m/z 253.1→117.1 (quantitative) and m/z 253.1→91.0 (qualitative).
TLC method was specific and durable. The linear range of 7, 4’-dihydroxyflavone was 0.470-37.58 ng·mL-1 (r=0.999 7) by UPLC-MS/MS. The average recovery rate(n=6) was 96.1% and RSD was 3.2%. Thirty batches of Zhenghonghua oil were screened by TLC, and 24 batches were suspected to have 7, 4’-dihydroxyflavone. The suspected samples were verified by UPLC-MS/MS, 24 batches of Zhenghonghua oil exceeded the proposed limit, and the verification results were consistent with TLC method.
This method is rapid, accurate and can be used for the screening and analysis of adulterated Zhenghonghua oil.
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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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