CN115304654A - 一种泰乐菌素的精制方法及所得产品的应用 - Google Patents
一种泰乐菌素的精制方法及所得产品的应用 Download PDFInfo
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Abstract
本发明公开了一种泰乐菌素的精制方法。本发明所述的泰乐菌素的精制方法：将泰乐菌素粗品与有机溶剂混合，降温至0～5℃，然后加入还原剂，在室温下搅拌1～2小时，过滤，在40℃下真空干燥，得到精制后的泰乐菌素纯品，所述的泰乐菌素纯品的纯度大于99％。本发明创造性的使用泰乐菌素作为抗支原体药物辅助药物，通过协同使用使得抗支原体药物作用更加明显。
Description
技术领域
本发明涉及化学技术领域，具体涉及一种泰乐菌素的精制方法，以及该方法所得产品的应用。
背景技术
泰乐菌素(Tylosin)，亦称泰农、泰乐霉素，是美国于1959年从弗氏链霉菌(Streptomyces fradiae)的培养液中获得的一种大环内酯类抗生素。泰乐菌素为一种白色板状结晶，微溶于水，呈碱性。产品有酒石酸盐、磷酸盐、盐酸盐、硫酸盐及乳酸盐，易溶于水。其水溶液在25℃、pH 5.5～7.5时可保存3个月，但是若水溶液中含有铁、铜等金属离子时，会使本品失效。
酒石酸泰乐菌素分子式为(C46H77NO17)2C4H6O5，分子量为1982.3。性状为白色或淡黄色粉末，易溶于水(600mg/ml)。因其肠道吸收好，体内扩散快，血药浓度高。
泰乐菌素常用来治疗家禽疾病。其临床应用方法较多，如片剂口服、粉剂饮水、肌肉注射、皮下注射、混饲给药、喷雾药浴等。酒石酸泰乐菌素在临床上主要用于治疗和预防由支原体、金黄葡萄球菌、化脓杆菌、肺炎双球菌、丹毒杆菌、副嗜血杆菌、脑膜炎奈瑟氏菌、巴氏杆菌、螺旋体、球虫等病原体引起的各种呼吸道、肠道、生殖道和运动系统感染。如：家禽慢性呼吸道病、鸡传染性鼻炎、禽气囊炎、传染性窦炎、输卵管炎、猪气喘病、萎缩性鼻炎、猪红痢、胃肠炎、猪丹毒、支原体关节炎、畜禽顽固性腹泻、坏死性肠炎、子宫内膜炎、家畜外生殖器化脓性感染、山羊胸膜肺炎、母羊流产、肉牛肝脓肿、牛羊腐蹄病等症。还用于种禽场进行种蛋注射、浸蛋等支原体净化。并且对预防和治疗畜禽在暴发病毒性疾病时支原体的继发感染有很好疗效，是世界公认治疗和预防畜禽支原体感染的首选药物，效果优于红霉素、北里霉素和泰妙菌素。
泰乐菌素如果能够合理的使用，将是很大的突破。同时，由于粗品泰乐菌素由于制备工艺复杂所以杂质非常多，无法直接应用，所以需要对其精制方法进行研究。
发明内容
发明目的，针对现有技术中的不足之处，本发明提供了一种泰乐菌素的精制方法，通过该方法得到的纯品泰乐菌素可以作为抗支原体药物辅助药物。
技术方案：本发明所述的泰乐菌素的精制方法：将泰乐菌素粗品与有机溶剂混合，降温至0～5℃，然后加入还原剂，在室温下搅拌1～2小时，过滤，在40℃下真空干燥，得到精制后的泰乐菌素纯品，所述的泰乐菌素纯品的纯度大于99％。
具体的，所述的有机溶剂为：甲醇、乙醇。
具体的，所述的还原剂为氰基硼氢化钠。
具体的，所述还原剂的加入量为粗品泰乐菌素质量的1.0％～1.5％。
本方法所得到的泰乐菌素纯品，纯度范围在99.4～99.7％之间。
有益效果：本发明通过使用氰基硼氢化钠创造性的精致获得泰乐菌素作为支原体药物辅助药物。
附图说明
图1为泰乐菌素粗品的纯度液相色谱图
图2为实施例1所得泰乐菌素纯品的液相色谱图
图3为实施例2所得泰乐菌素纯品的液相色谱图
图4为实施例3所得泰乐菌素空白实验的液相色谱图
具体实施方式
下面是实施例对本发明方案进行详细说明，但是本发明的保护范围不局限于所述实施例。
实施例1
泰乐菌素粗品(含量96.512％)10克和100克甲醇加入500毫升圆底烧瓶中，降温到0-5度后，分3次加入1克的氰基硼氢化钠，室温下搅拌1个小时，过滤并在50度下真空干燥12小时得到泰乐菌素纯品8.6克收率86％；纯度大于99.674％。色谱图见图2，数据见下表
检测器A 214nm
| Peak# | Ret.Time | Area | Height | 面积％ | Conc. | Unit |
| 1 | 3.600 | 44751 | 5051 | 0.180 | 0.180 | |
| 2 | 3.876 | 3081 | 414 | 0.019 | 0.019 | |
| 3 | 4.226 | 15886874 | 1606650 | 99.674 | 99.674 | |
| 4 | 6.080 | 4291 | 385 | 0.027 | 0.027 | |
| 5 | 6.863 | 3605 | 287 | 0.023 | 0.023 | |
| 6 | 7.361 | 1221 | 95 | 0.008 | 0.008 | |
| 7 | 19.341 | 10634 | 434 | 0.067 | 0.067 | |
| 8 | 22.669 | 10720 | 467 | 0.067 | 0.067 | |
| 9 | 22.875 | 3862 | 352 | 0.024 | 0.024 | |
| 10 | 24.247 | 2392 | 182 | 0.015 | 0.015 | |
| 11 | 24.492 | 1081 | 159 | 0.007 | 0.007 | |
| 总计 | 15972511 | 1614477 | 100.000 |
实施例2
泰乐菌素粗品(含量96.512％)10克和100克乙醇加入500毫升圆底烧瓶中，降温到0-5度后，分3次加入1克的氰基硼氢化钠，室温下搅拌2个小时，过滤并在50度下真空干燥12小时得到泰乐菌素纯品8.9克收率89％；纯度大于99.464％。色谱图见图3，数据见下表
检测器A 214nm
| Peak# | Ret.Time | Area | Height | 面积％ | Conc. | Unit |
| 1 | 3.600 | 44751 | 5051 | 0.280 | 0.280 | |
| 2 | 3.876 | 3081 | 414 | 0.019 | 0.019 | |
| 3 | 4.226 | 15886874 | 1606650 | 99.464 | 99.464 | |
| 4 | 6.080 | 4291 | 385 | 0.027 | 0.027 | |
| 5 | 6.863 | 3605 | 287 | 0.023 | 0.023 | |
| 6 | 7.361 | 1221 | 95 | 0.008 | 0.008 | |
| 7 | 19.341 | 10634 | 434 | 0.067 | 0.067 | |
| 8 | 22.669 | 10720 | 467 | 0.067 | 0.067 | |
| 9 | 22.875 | 3862 | 352 | 0.024 | 0.024 | |
| 10 | 24.247 | 2392 | 182 | 0.015 | 0.015 | |
| 11 | 24.492 | 1081 | 159 | 0.007 | 0.007 | |
| 总计 | 15972511 | 1614477 | 100.000 |
实施例3
(不添加氰基硼氢化钠的空白实验)泰乐菌素粗品(含量96.512％)10克和100克乙醇加入500毫升圆底烧瓶中，降温到0-5度后，又室温下搅拌2个小时，过滤并在50度下真空干燥12小时得到泰乐菌素纯品9.9克收率99％；纯度96.912％。色谱图见图4，数据见下表
检测器A 214nm
| Peak# | Ret.Time | Area | Height | 面积％ | Conc. | Unit |
| 1 | 2.978 | 71287 | 5899 | 0.313 | 0.313 | |
| 2 | 3.607 | 202610 | 22760 | 1.431 | 1.431 | |
| 3 | 4.228 | 13668896 | 1410020 | 96.912 | 96.912 | |
| 4 | 7.237 | 5171 | 332 | 0.037 | 0.037 | |
| 5 | 16.184 | 148841 | 2561 | 1.051 | 1.051 | |
| 6 | 19.283 | 7422 | 285 | 0.052 | 0.052 | |
| 7 | 22.698 | 43870 | 1228 | 0.310 | 0.310 | |
| 8 | 24.200 | 14838 | 452 | 0.105 | 0.105 | |
| 总计 | 14162934 | 1443537 | 100.000 |
以上所述仅为本申请的优选实施例而已，并不用于限制本申请。
Claims (4)
1.一种泰乐菌素的精制方法，其特征在于，将泰乐菌素粗品与有机溶剂混合，降温至0～5℃，然后加入还原剂，在室温下搅拌1～2小时，过滤，在40℃下真空干燥，得到精制后的泰乐菌素纯品，所述的泰乐菌素纯品的纯度大于99％。
2.根据权利要求1所述的泰乐菌素的精制方法，其特征在于，所述的有机溶剂为：甲醇、乙醇。
3.根据权利要求1所述的泰乐菌素的精制方法，其特征在于，所述的还原剂为氰基硼氢化钠。
4.根据权利要求1所述的泰乐菌素的精制方法，其特征在于，所述还原剂的加入量为粗品泰乐菌素质量的1.0％～1.5％。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211739A (zh) * | 2013-09-29 | 2014-12-17 | 郑州后羿制药有限公司 | 一种泰乐菌素的精制方法 |
| CN104558076A (zh) * | 2015-02-10 | 2015-04-29 | 上海皓元化学科技有限公司 | 一种泰地罗新的制备方法及其中间体化合物 |
| CN108264530A (zh) * | 2016-12-30 | 2018-07-10 | 湖北回盛生物科技有限公司 | 20,23-二卤代-5-o-碳霉胺糖基-泰乐内酯及其合成方法和应用 |
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| CN104211739A (zh) * | 2013-09-29 | 2014-12-17 | 郑州后羿制药有限公司 | 一种泰乐菌素的精制方法 |
| CN104558076A (zh) * | 2015-02-10 | 2015-04-29 | 上海皓元化学科技有限公司 | 一种泰地罗新的制备方法及其中间体化合物 |
| CN108264530A (zh) * | 2016-12-30 | 2018-07-10 | 湖北回盛生物科技有限公司 | 20,23-二卤代-5-o-碳霉胺糖基-泰乐内酯及其合成方法和应用 |
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