Method for detecting lignans and flavonol glycoside compounds in ginkgo biloba extract or preparation of ginkgo biloba extract
A flavonol glycosides and detection method technology, applied in the field of detection of ginkgo biloba extract, can solve the problems of simultaneous quantitative detection and other problems, improve and control quality, simplify the inspection process, and have good reproducibility and stability Effect
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Embodiment 1
[0030] Materials and Methods
[0031] Instrument: Waters Xevo GX-XS quadrupole tandem time-of-flight mass spectrometer
[0032] Reagents: acetonitrile, methanol (chromatographically pure), purified water, and other reagents are of analytical grade; agaricin-4,4-diglucoside, pinoresinol diglucoside, Urolignoside and cosmoside reference substances
[0033] Samples: Ginkgo biloba extract, Shuxuening injection
[0034] Solution preparation:
[0035] Preparation of reference solution:
[0036] Precisely weigh 12.16mg of agaricin-4,4-diglucoside in a 50ml volumetric flask, 10.90mg of pinoresinol diglucoside in a 50ml volumetric flask, 9.20mg of Urolignoside in a 50ml volumetric flask, and 10.26mg of cosmoside in a 50ml volumetric flask bottle, dissolved in methanol and made to volume, as the mother solution of the reference substance. Precisely measure 2ml of agaricin-4,4-diglucoside, 2ml of pinoresinol diglucoside, 5ml of Urolignoside and 1ml of cosmoside reference substance mo...
Embodiment 2
[0046] Methodological investigation and results
[0047] Linear relationship: Dilute the mixed reference solution 2 times, 5 times, 10 times, 20 times and 40 times respectively, precisely draw 1 μL of the mixed reference solution and the above-mentioned diluted solution into the liquid chromatograph, and extract each component to be tested The exact molecular weight was recorded and the peak area was recorded.
[0048] Wherein, the results of linear relationship investigation of agaricin-4,4-diglucoside are shown in Table 1;
[0049] Table 1 Investigation of the linear relationship of agaricin-4,4-diglucoside
[0050]
[0051]
[0052] According to the above table, with the injection volume (ug) as the abscissa (X), and the peak area as the ordinate (Y), draw a standard curve to obtain the regression equation of agaricin-4,4-diglucoside as:
[0053] y=23574.7465x+35594.1644, R2=0.9997 (n=6). It shows that agaricin-4,4-diglucoside in the reference substance has a good li...
Embodiment 3
[0102] The UPLC-MS method in Example 1 was used to detect the contents of agaricin-4,4-diglucoside, pinoresinol diglucoside, Urolignoside and cosmoside in the Ginkgo biloba extract.
[0103] Get 10 batches of Ginkgo biloba extracts, 2 parts per batch, prepare the solution to be tested according to the preparation method of the Ginkgo biloba extract test solution in Example 1, accurately draw 1ul into the chromatograph, and extract the precise molecular weight of each component to be tested , record the peak area, and calculate the content of each component to be tested in the Ginkgo biloba extract, and the content detection results are shown in Table 15-18.
[0104] Table 15 Determination results of agaricin-4,4-diglucoside content in Ginkgo biloba extract
[0105]
[0106]
[0107] Determination results of pinoresinol diglucoside content in table 16 Ginkgo biloba extract
[0108]
[0109]
[0110] Table 17 Determination results of Urolignoside content in Ginkgo b...
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