Heparin calcium

White or almost white, hygroscopic powder.

The method using crude heparin sodium as the raw material—decolorization, precipitation, and dissolution. Dissolve the crude heparin sodium (above 80U/mg) in 15 times the amount of 2% NaCl solution, adjust the pH to about 8 with 4mol/L NaOH solution, and heat at 80°C. Add 1mol KMnO4 to 100 million units of crude heparin sodium, keep for 30min, filter to remove MnO2, adjust the pH of the filtrate to 6.4 with 6mol/L HCl, add 0.8 times the amount of ethanol to the volume of the filtrate, leave it for 12h, suck off the supernatant and precipitate Dissolve with ion-free water, filter by suction through a layer of talc, and collect the filtrate. Crude heparin sodium [2%NaCl, NaOH, KMnO4]→[pH8, 80℃] decolorization filtrate [HCl, ethanol]→[pH6.4, 12h] precipitate [deionized water]→separation, neutralization, Precipitate and dry the above heparin sodium solution. Add a certain proportion of 732 type cation exchange resin. After stirring for half an hour, the resin is removed. The solution is adjusted to pH 7.8 with calcium oxide solution. Add an appropriate amount of anhydrous calcium chloride, filter by suction, and press the volume of the filtrate. Add 0.8 times the amount of ethanol and let it stand overnight in a cold storage below 10°C. The supernatant was aspirated the next day, the precipitate was washed with absolute ethanol and acetone, dehydrated, drained, and dried in a P2O5 vacuum dryer to obtain heparin calcium premium. The potency yield is 90% to 92%, and the product quality meets the full requirements of the BP1980 version. Heparin sodium solution [732 resin]→[30min] heparin solution [CaO, CaCl2]→[pH7.8] filtrate [ethanol]→[10℃below, 24h] precipitate [absolute ethanol, acetone]→heparin calcium boutique Method using crude heparin sodium as raw material 2 Take 292g crude heparin sodium (125U/mg), add 3L 4mol/L NaCl solution, adjust pH9 with 20% NaOH solution, keep it at 60℃ for 1h, heat up to a slight boiling for 15min, and filter. The precipitation was extracted once more with 500ml 4mol/L NaCl solution in the same way. Combine the filtrate, add 2 times the volume of ethanol to precipitate after cooling, filter, soak the precipitate with 500ml alcohol solution alcohol (V): water (V)=2:1 for 2h, filter, and wash twice with the same proportion of alcohol. Crude sodium heparin [NaCl]→solution [NaOH]→[pH9, 60℃, 1h] filtrate [ethanol]→precipitation The above precipitate is dissolved in 2L of water, and passed through a pre-treated cation exchange resin (H+) column that has been washed to neutrality. Then wash with 1L of water, combine the effluents, and filter to remove insolubles. Add CaCl2 to a solution concentration of 1mol/L, add calcium oxide water to pH11, add H2O2 to a content of 2%, oxidize for 2h, after filtration, adjust the pH to 6.5 with 6mol/L HCl, and add to 1.5 times the volume of ethanol to precipitate . Precipitation [water]→solution [cation resin]→effluent [CaCl2, CaO, H2O2, HCl]→[pH11, pH6.5] filtrate [ethanol]→precipitate the above precipitation and dissolve it with 1.5L, 0.1mol/L CaCl2 solution, Adjust the pH to 7.0-7.5 with CaO and let it stand overnight. After filtration, the filtrate is adjusted to pH 6.5, added to 2 times volume of ethanol for precipitation, filtered, washed, and dried to obtain 200 g of heparin calcium. The specific activity is 150U/mg, and the yield is 82.19%. Precipitation [CaCl2, CaO]→[pH7.0-7.5] filtrate [ethanol]→[pH6.5] heparin calcium.

Used as an anticoagulant