High-purity antibiotic medicinal compound
A technology of pharmaceutical compounds and antibiotics, applied in the field of medicine, can solve problems affecting clinical application, decreased stability of preparations, low purity, etc., and achieve the effects of improving clinical drug effects, improving stability, and low cost
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Embodiment 1
[0035] The refining of embodiment 1 azlocillin sodium
[0036] (1) Dissolve 100g of azlocillin sodium in 1000ml of water, add 1mol / L hydrochloric acid solution to adjust the pH value to 3.0, stir to precipitate insoluble matter, filter, and obtain a solid after washing with purified water;
[0037] (2) Dissolve the solid obtained in step (1) with 1500ml of a mixture of ethanol and acetone (5:1), add to the column filled with D101 macroporous resin and pass through, then use chloroform and isopropanol (3:1) mixture 500ml for elution and purification, and collect the eluate;
[0038] (3) The eluate obtained in step (2) is adjusted to a pH value of 5.5 with 10% sodium acetate solution, and a solid is precipitated, centrifuged for 10 min, washed with 500 ml of isopropanol, and vacuum-dried at 50° C. for 5 hours to obtain a refined product of 94.5 g, the yield is 94.5%, and the HPLC detection purity is 99.96%.
Embodiment 2
[0039] The refining of embodiment 2 mezlocillin sodium
[0040](1) 100g mezlocillin sodium is dissolved in 1000ml water, the phosphoric acid solution that adds 5mol / L is adjusted pH value is 4.0, stirs and separates out insoluble matter, filters, obtains solid after purified water washing;
[0041] (2) Dissolve 1300ml of the solid obtained in step (1) with a mixture of ethanol and acetone (5:1), add to the column filled with AB-8 macroporous resin and pass through, then use chloroform and isopropanol (3:1) ) 600ml of the mixture was eluted and purified, and the eluate was collected;
[0042] (3) Adjust the pH value of the eluate obtained in step (2) to 7.0 with 10% sodium citrate solution, and precipitate a solid, centrifuge for 20 minutes, wash with 500ml of isopropanol, and vacuum-dry at 60°C for 3 hours to obtain the essence The product is 92.8g, the yield is 92.8%, and the purity detected by HPLC is 99.94%.
Embodiment 3
[0043] The refining of embodiment 3 piperacillin sodium
[0044] (1) 100g of piperacillin sodium is dissolved in 800ml of water, and the nitric acid solution of 2mol / L is added to adjust the pH value to 3.5, and the insoluble matter is precipitated by stirring, filtered, and washed with purified water to obtain a solid;
[0045] (2) Dissolve 1200ml of the solid obtained in step (1) with a mixture of ethanol and acetone (5:1), add to the column filled with AB-8 macroporous resin and pass through, then use chloroform and isopropanol (3:1) ) 500ml of the mixture was eluted and purified, and the eluate was collected;
[0046] (3) The eluent obtained in step (2) is adjusted to a pH value of 6.0 with 0.1mol / L sodium hydroxide solution, and a solid is precipitated, centrifuged for 10 min, washed with 500 ml of isopropanol, and vacuum-dried at 55° C. for 4 hours to obtain The refined product is 93.7g, the yield is 93.7%, and the purity detected by HPLC is 99.93%.
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