A detection method for simultaneously determining the content of flavonoids and terpene lactones in ginkgo biloba extract and its preparations
A technology of ginkgolide and ginkgo biloba, applied in the field of high-performance liquid chromatography detection, can solve the problems of insufficient process simplicity and complicated operation steps, and achieve the effect of low cost, good durability and easy realization
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Embodiment 1
[0038](1) Chromatographic conditions: the stationary phase is a chromatographic column filled with octadecyl bonded silica gel; the UV detector is connected in series with the ELSD detector; the UV detection wavelength is 360nm; the flow rate is 1mL / min; the mobile phase A is 0.05% tetrahydrofuran -0.1% formic acid-5% methanol-water mixed solvent, the volume ratio is 1:2:10:950; mobile phase B is a mixed solvent of 0.1% tetrahydrofuran-methanol-acetonitrile solution, the volume ratio is 1:1000, wherein Methanol-acetonitrile solution is a solution with a volume ratio of methanol and acetonitrile of 1:1; gradient elution is performed, and the gradient conditions are:
[0039] time (min)
A(%)
B(%)
0~10
90→84
10→16
10~30
84→80
16→20
30~33
80→79
20→21
33~47
79→79
21→21
47~48
79→76
21→24
48~63
76→67
24→33
63~64
67→60
33→40
64~74
60→45
40→55
74~75
45→90
55→10 ...
Embodiment 2
[0054] Embodiment 2: Ginkgo biloba sample content detection method
[0055] (1) Sample preparation: Take 8 batches of Ginkgo biloba sample powder, weigh 1g precisely, put it in a 10ml volumetric flask, add 70% methanol solution to set the scale mark, and extract by ultrasonic for 30min. The extract was centrifuged at a speed of 14000r / min for 10min, and the supernatant was taken, and then centrifuged at a speed of 14000r / min for 10min, and the supernatant was taken. Take 1ml of the supernatant and blow it with nitrogen to redissolve to 250ul to increase the sample concentration by 4 times, and store it in a refrigerator at 4°C as a stock solution of ginkgo biloba leaves for later use.
[0056] (2) Content detection
[0057] According to the chromatographic conditions described in Example 1, the sample was injected, the peak area was measured, and the corresponding standard line was substituted to calculate the contents of the 11 compounds in the ginkgo biloba sample. The tes...
Embodiment 3
[0060] Embodiment 3: Shuxuening injection content detection method
[0061] (1) Sample preparation: Shuxuening injection was heated at 14000r.min -1 Centrifuge at a high speed for 10min, take the supernatant, and re-centrifuge the supernatant at 14000r.min -1 centrifuge for 10 min at a high speed, take the supernatant, and store it in a refrigerator at 4°C as the stock solution of the Shuxuening injection sample for later use.
[0062] (2) Content detection
[0063] According to the chromatographic conditions described in Example 1, the sample was injected, the peak area was measured, and the corresponding standard line was substituted to calculate the contents of the 11 compounds in the ginkgo biloba sample. The test results of the samples are shown in Table 4.
[0064] Table 4 Shuxuening injection content assay results
[0065]
[0066]
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