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To analyze the chemical constituents of Quyusanjie capsules by LC/MS, and establish a method for the determination of active ingredients in Quyusanjie capsules.
Using UPLC-Q TOF MS/MS technology, the Hypersil Gold C18 column(100 mm×2.1 mm, 1.9 μm) was used, the mobile phase was acetonitrile(A) and 0.1% formic acid in water(B) with gradient elution, at a flow rate of 0.4 mL·min-1, the the column temperature was 40.0 ℃, and the mass spectrometry data was collected by negative ions mode scanning. Through database matching, elemental composition and fragment structure analysis, the main chemical substances in Quyusanjie capsules were identified. HPLC was used to qualitatively analyze the chemical components of Quyusanjie capsules. The Ultimate® AQ-C18 column(250 mm×4.6 mm, 5 μm) was used, the mobile phase was acetonitrile(A) -0.1% phosphoric acid(B) with gradient elution at the flow rate of 1.0 mL·min-1, the column temperature was 25 ℃, and the detection wavelength was 203 nm. The content of naringin, neohesperidin, notoginsenoside R1, ginsenoside Rg1, and ginsenoside Rb1 in 11 different batches of Quyusanjie capsules were determined using external standard method. QAMS method was established using ginsenoside Rg1 as the internal reference.
Twenty-nine compounds were identified from Quyusanjie capsule. The contents of naringin, neohesperidin, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 measured by external standard method were 0.484-1.097 mg·g-1, 0.341-0.618 mg·g-1, 1.685-2.399 mg·g-1, 5.748-8.386 mg·g-1, 3.868-5.898 mg·g -1, respectively. Measured with the QAMS method, the contents of naringin, neohesperidin, notoginsenoside R1 and ginsenoside Rb1 were 0.516-1.153 mg·g-1, 0.372-0.667 mg·g-1, 1.794-2.580 mg·g-1, 4.373-6.690 mg·g-1, respectively. The relative error between the calculated values of the QAMS method and the measured value of the external standard method was less than 8.9%.
UPLC-Q TOF MS/MS method can quickly identify the chemical components of Quyusanjie capsules. The established external standard method is stable and reliable, and can be used for the quality control of Quyusanjie capsules. The method of QAMS has good feasibility and is suitable for the determination of the daily production of Quyusanjie capsules.
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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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