Doxycycline injection and preparation method thereof
A technology of doxycycline and doxycycline hydrochloride, which is applied in the field of animal injections, can solve the problems that the development level needs to be further improved, and achieve the effect of good stability
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Embodiment 1
[0031] (1) Preparation of doxycycline magnesium N-acetylglycinate
[0032] a. Dissolve 100 g (0.195 mol) of doxycycline hydrochloride in 500 mL of water;
[0033] b. Add magnesium chloride hexahydrate 39.6g (0.195mol), stir and dissolve;
[0034] c. Add 22.8g (0.195mol) of N-acetylglycine and stir to dissolve;
[0035] d. 1000 mL of ethanol was added dropwise, stirred overnight, and a crystalline solid was precipitated, filtered, and vacuum-dried to obtain 116 g of doxycycline magnesium N-acetylglycinate.
[0036] (2) Preparation of doxycycline injection
[0037] Weigh 10.6g of doxycycline magnesium N-acetylglycinate, 0.2g of sodium bisulfite, 0.2mL of benzyl alcohol, 50mL of α-pyrrolidone, and make up to 100mL of propylene glycol according to the formula, mix well and filter to make 10mL / An ampoule bottle filled with nitrogen, sealed and sterilized for doxycycline injection.
Embodiment 2
[0039] (1) Preparation of doxycycline zinc N-acetylthreonine salt
[0040] a. Dissolve 100 g (0.195 mol) of doxycycline hydrochloride in 500 mL of water;
[0041] b. Add anhydrous zinc chloride 26.6g (0.195mol), stir and dissolve;
[0042] c. Add 31.4 g (0.195 mol) of N-acetylthreonine and stir to dissolve;
[0043] d. 700 mL of methanol was added dropwise, stirred overnight, and a crystalline solid was precipitated, filtered, and vacuum-dried to obtain 120 g of doxycycline zinc N-acetylthreoninate.
[0044] (2) Preparation of doxycycline injection
[0045] Weigh 11.2g of doxycycline zinc N-acetylthreoninate, 0.2g of diaobaikuai, 0.2mL of benzyl alcohol, 50mL of N-methylpyrrolidone, and polyethylene glycol 300 to 100mL according to the formula, and mix well After filtering, make 10mL / support ampoule bottle, fill with nitrogen, fill and seal, sterilize doxycycline injection.
Embodiment 3
[0047] (1) Preparation of doxycycline calcium N-acetylglycine salt
[0048] a. Dissolve 100 g (0.195 mol) of doxycycline hydrochloride in 500 mL of water;
[0049] b. Add 28.7g (0.195mol) of calcium chloride dihydrate and stir to dissolve;
[0050] c. Add 22.8g (0.195mol) of N-acetylglycine and stir to dissolve;
[0051] d. 1200 mL of isopropanol was added dropwise, stirred overnight, and a crystalline solid was precipitated, filtered, and vacuum-dried to obtain 116 g of doxycycline calcium N-acetylglycinate.
[0052] (2) Preparation of doxycycline injection
[0053] Weigh 10.9g of doxycycline calcium N-acetylglycinate, 0.2g of sodium metabisulfite, 0.2g of benzoic acid, 50mL of N,N-dimethylacetamide, and polyethylene glycol 400 to make up to 100mL, mix After homogenization, filter to make 10mL / ampoules, fill with nitrogen, fill and seal, and sterilize doxycycline injection.
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