To establish a method for qualitative and quantitative determination of Asini Corii Colla in Ejiao Yishou oral liquid by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).
The Ejiao Yishou oral liquid sample was digested with trypsin prior to HPLC-MS/MS analysis. A ZORBAX Eclipse Plus C18 column (3.0 mm×150 mm, 1.8 μm) was adopted, using 0.1% formic acid aqueous solution-acetonitrile as mobile phase for gradient elution. Under the electrospray ionization mode, multi-reaction monitoring was carried out and the specific identification of Asini Corii Colla and the determination of the content of characteristic peptides of Asini Corii Colla were conducted.
The polypeptides derived from Asini Corii Colla exhibited good linearity relationships, with all correlation coefficients above 0.999. The relative standard deviations for instrumental precision,sample stability and method repeatability were all less than 4.0%, and the spiked recoveries at 3 concentration levels ranged from 88.30% to 100.22%. Asini Corii Colla was detected in all 126 batches of samples, while 91.3% of the samples had total content of the donkey-derived peptide A1 and peptide A2 below the proposed limit.
The established method is accurate, reliable and highly specific, and can be used for the quality control of Asini Corii Colla in the Ejiao Yishou oral liquid.
| 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 |