A low anticoagulant heparin, its oligosaccharides, its preparation method and its application in the preparation of anti-Alzheimer's disease medicine
A low anticoagulant and oligosaccharide technology, applied in the field of medicine, can solve the problems of waste of biological resources, low anticoagulant heparin by-products, etc., and achieve low cost, abundant raw material sources, and good anti-Alzheimer's effect
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Embodiment 1
[0034] Example 1: Preparation of low anticoagulant heparin
[0035] The preparation method of low anticoagulant heparin of the present invention specifically comprises the following steps:
[0036] 1. Chondroitinase ABC enzyme removes chondroitin impurities: dissolve pig intestinal mucosa crude heparin (10g) purchased from a heparin production plant in 3L enzymolysis buffer (0.05mol L -1 Ammonium acetate, 2mmol·L -1 Calcium chloride), 50 Units of chondroitinase ABC were added thereto, reacted on a shaking table at 35° C. for 6 hours, and inactivated in a boiling water bath for 10 minutes.
[0037] 2. Hydrochloric acid precipitation to remove nucleic acid impurities: centrifuge the enzymatic solution and take the supernatant. Add 1 mol·L dropwise to the supernatant with stirring -1 hydrochloric acid until the pH of the enzymolysis solution is 3.0, centrifuge, take the supernatant and use 1mol·L -1 neutralized to pH 7.0 with NaOH.
[0038] 3. Ethanol precipitation: After co...
Embodiment 2
[0040] Example 2: Structural characterization of the low anticoagulant heparin
[0041](1) Absolute molecular weight determination and purity analysis: The absolute molecular mass of the low anticoagulant heparin was determined and the purity was analyzed by high performance gel permeation chromatography (HPGPC)-octadecanine laser light scattering method (MALLs).
[0042] Chromatographic conditions: Column: Shodex OHPak SB804HQ column connected in series with Shodex OHPak SB802.5HQ column; mobile phase: 0.1mol L -1 Na 2 SO 4 Aqueous solution; The molecular weight of low anticoagulant heparin is detected and determined in series by a differential detector and an octagonal laser light scattering instrument in series; the sample is in the middle of a single symmetrical peak in the HPGPC spectrogram (such as figure 1 Shown), the sample purity is very high, and its absolute molecular mass is measured as 10.24kDa.
[0043] (2) Analysis of disaccharide composition: make low antico...
Embodiment 3
[0049] Example 3: Anticoagulant activity of low anticoagulant heparin
[0050] Follow the steps indicated in the kit to determine the inhibitory effect of the sample on the activity of FXa and FIIa, the initial concentration of the sample is 0.001, 0.01, 0.1, 1, 10 and 100 μg·mL -1 . Add 20 μL antithrombin III (ATIII) and 20 μL sample solution to each well of the 96-well plate, incubate at 37°C for 1 min, then add 40 μL FXa or FIIa, incubate at 37°C for 1 min, add 100 μL FXa or FIIa substrate, 37 Incubate at ℃ for 4min, finally add 100μL of stop solution, detect the absorbance at 405nm wavelength, and calculate the inhibition rate: the result ( Figure 4 ) showed that LAH had weak anticoagulant activity, which was much lower than that of HP and ES standards, and slightly higher than that of HS standards.
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