CN1813785A - 一种盐酸克林霉素粉针剂的制备方法 - Google Patents
一种盐酸克林霉素粉针剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种盐酸克林霉素粉针剂的制备方法,包括以下几个步骤:(1)盐酸克林霉素,加溶剂溶解;(2)溶解后的溶液脱色,过滤;(3)将上述滤液在无菌环境下,精滤得精滤液;(4)精滤液加入丙酮升温至溶解,加入活性炭,趁热过滤;(5)加入丙酮后,放置得盐酸克林霉素结晶体;(6)将盐酸克林霉素结晶体烘干,粉碎,分装。利用本发明公开的方法可以得到稳定的盐酸克林霉素粉针剂。
Description
技术领域
本发明属于一种药物制剂的制备方法,特别涉及一种治疗革兰氏阳性菌引起的感染性疾病和厌氧菌引起的感染性疾病的制剂的制备方法。
背景技术
盐酸克林霉素是由林可霉素7位上的羟基被氯取代后所得的衍生物,最早由Magerlein等人于1966年合成,本品为林可霉素类抗生素,抗菌活性较林可霉素强4~8倍。克林霉素通过与核糖体50S亚基结合,阻止肽链的延长,抑制细菌蛋白质的合成。对革兰阳性菌如葡萄球菌属(包括耐青霉素株)、链球菌属、大肠杆菌、破伤风杆菌、肺炎球菌及魏氏梭菌、少数放线杆菌有极好的疗效,对支原体也有效,对耐青霉素、红霉素等药物的病原微生物仍有高效,与青霉素、头孢霉素、四环素等其它抗生素无交叉耐药现象。对革兰阴性厌氧菌也有良好抗菌活性,拟杆菌属包括脆弱拟杆菌、梭杆菌属、消化球菌、消化链球菌、产气荚膜杆菌等大多对本品高度敏感。本品系抑菌药,但在高浓度时,对某些细菌也具有杀菌作用。本品适用于链球菌、葡萄球菌、支原体等敏感菌引起的呼吸道感染、传染性胸膜肺炎、子宫内膜炎、乳房炎等。对耐其它药物细菌引起的痢疾、喘气及支原体疾病,克林霉素更为适宜。
盐酸克林霉素在水溶液中稳定性较差,有许多降解产物其结构及药理性质尚不清楚,有可能会影响用药安全,其注射液需要在阴凉处保存,给运输、贮存造成不便。盐酸克林霉素水针剂在制备过程中加入了一定量的等渗剂、pH值调节剂、抗氧剂等附加剂,产品需高温灭菌,增加了盐酸克林霉素的降解,产品的安全性降低,影响了产品的稳定性。冻干制剂比注射液稳定,容易贮存、运输,对保证药品的质量有利,但成本高,因此,临床上急需开发出价廉稳定的盐酸克林霉素制剂。
发明内容
本发明公开了:
1.一种盐酸克林霉素粉针剂的制备方法,包括以下步骤:
(1)盐酸克林霉素加溶剂溶解;
(2)溶解后的溶液脱色,过滤;
(3)将上述滤液在无菌环境下,精滤得精滤液;
(4)精滤液加入丙酮升温至溶解,加入活性炭,趁热过滤;
(5)加入丙酮后,放置得盐酸克林霉素结晶体;
(6)将盐酸克林霉素结晶体烘干,粉碎,分装。
2.上述1所述的方法,其中步骤(1)中溶剂为水或乙醇之一。
3.上述1所述的方法,其中步骤(2)中脱色剂为活性炭。
4.上述1所述的方法,其中步骤(3)中精滤用微孔滤膜或/和垂溶漏斗或/和微孔滤器或/和超滤器。
5.上述1所述的方法,其中步骤(6)在无菌环境下分装,轧盖,包装即得。
6.上述1所述的方法,其中在进行步骤(6)前对步骤(5)得到的盐酸克林霉素结晶体再进行第二次转溶、重结晶一次,得到重结晶的盐酸克林霉素结晶体。
本发明的盐酸克林霉素粉针剂的制备方法采用溶媒结晶法和先进的无菌分装技术,制备过程中无需高温处理,不需加入附加剂,制备过程用水量少,用本发明制成的盐酸克林霉素粉针剂不需要灭菌,减少了水解和降解反应的发生,产品粉末流动性好、纯度高、杂质少、生物得用度高、稳定性好。
经稳定性试验(是否还需要补充数据?)研究表明,制备工艺稳定可行。安全性试验表明本发明盐酸克林霉素粉针剂不产生过敏反应和溶血作用,静脉注射对血管无刺激性。(是否还需要补充数据?)
本发明克服了已有的盐酸克林霉素剂型的不足之处,提高了盐酸克林霉素的稳定性,满足了药物的临床需要。
具体实施方式
以下实施例仅对本发明进行进一步的说明,不应理解为对本发明的进一步的限制。
原材料来源:盐酸克林霉素
其它如果没有特别说明,均为市售。
实施例1:盐酸克林霉素粉针剂的制备(规格:600mg/支)
取处方量的盐酸克林霉素,加入70℃注射用水800ml,搅拌使溶解,加入针用活性炭3%,搅拌吸附30分钟,用硅藻土过滤器和钛过滤器粗滤后,在无菌环境(局部100级)下,用0.45μm的过滤器精滤,滤液加入丙酮3500ml升温至55℃溶解,加入活性炭100g,趁热用垂溶漏斗过滤,在搅拌下加入丙酮8000ml于洁净室内5-10℃放置结晶,用垂熔漏斗过滤后,80℃烘干,粉碎,在无菌环境(局部100级)下分装,成600mg/支,轧盖,包装即得。
实施例2:盐酸克林霉素粉针剂的制备(规格:600mg/支)
取处方量的盐酸克林霉素,加入60℃乙醇900ml,搅拌使溶解,加入针用活性炭3%,搅拌吸附25分钟,用硅藻土过滤器和钛过滤器粗滤后,在无菌环境(局部100级)下,用0.45μm的微孔滤膜精滤,滤液加入丙酮4000ml升温至50℃溶解,加入活性炭150g,趁热用垂溶漏斗过滤,在搅拌下加入丙酮8000ml于洁净室内5-10℃放置结晶,用垂熔漏斗过滤后83℃烘干,粉碎,在无菌环境(局部100级)下分装,成600mg/支,轧盖,包装即得。
实施例3:盐酸克林霉素粉针剂的制备(规格:600mg/支)
取处方量的盐酸克林霉素,加入75℃注射用水750ml,搅拌使溶解,加入针用活性炭3.5%,搅拌吸附25分钟,用硅藻土过滤器和钛过滤器粗滤后,在无菌环境(局部100级)下,用0.45μm的过滤器精滤,滤液加入丙酮3500ml升温至55℃溶解,加入活性炭100g,趁热用垂溶漏斗过滤,在搅拌下加入丙酮8000ml于洁净室内5-10℃放置结晶,用垂熔漏斗过滤后,80℃烘干,粉碎,在无菌环境(局部100级)下分装,成600mg/支,轧盖,包装即得。
实施例4:盐酸克林霉素粉针剂的制备(规格:600mg/支)
取处方量的盐酸克林霉素,加入70℃注射用水800ml,搅拌使溶解,加入针用活性炭3%,搅拌吸附30分钟,用硅藻土过滤器和钛过滤器粗滤后,在无菌环境(局部100级)下,用0.45μm的过滤器精滤,滤液加入丙酮3500ml升温至55℃溶解,加入活性炭100g,趁热用垂溶漏斗过滤,在搅拌下加入丙酮8000ml于洁净室内5-10℃放置结晶,过滤然后加入70℃注射用水800ml重新溶解后在搅拌下加入再次丙酮8000ml于洁净室内5-10℃放置结晶,用垂熔漏斗过滤后,80℃烘干,粉碎,在无菌环境(局部100级)下分装,成600mg/支,轧盖,包装即得。
Claims (6)
1.一种盐酸克林霉素粉针剂的制备方法,包括以下步骤:
(1)盐酸克林霉素加溶剂溶解;
(2)溶解后的溶液脱色,过滤;
(3)将上述滤液在无菌环境下,精滤得精滤液;
(4)精滤液加入丙酮升温至溶解,加入活性炭,趁热过滤;
(5)加入丙酮后,放置得盐酸克林霉素结晶体;
(6)将盐酸克林霉素结晶体烘干,粉碎,分装。
2.权利要求1所述的方法,其中步骤(1)中溶剂为水或乙醇之一。
3.权利要求1所述的方法,其中步骤(2)中脱色剂为活性炭。
4.权利要求1所述的方法,其中步骤(3)中精滤用用微孔滤膜或/和垂溶漏斗或/和微孔滤器或/和超滤器。
5.权利要求1所述的方法,其中步骤(6)在无菌环境下分装,包装即得。
6.权利要求1所述的方法,其中在进行步骤(6)前对步骤(5)得到的盐酸克林霉素结晶体再进行第二次转溶、重结晶一次,得到重结晶的盐酸克林霉素结晶体。
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