CN106290625A - 一种地红霉素原料有关物质的检测方法 - Google Patents
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Abstract
本发明提供一种地红霉素原料有关物质的检测方法。该方法是采用高效液相色谱法进行的,包括下述步骤:(1)配制地红霉素样品溶液(2)将步骤;(1)所得样品溶液注入高效液相色谱仪,并记录色谱图;其中,所述高效液相色谱法的色谱柱固定相填充剂为十八烷基硅烷键合硅胶;流动相的配制为水:甲醇:乙腈:磷酸盐缓冲溶液=14:19:39:28;本发明的检测方法在同一液相条件下测定地红霉素原料中的有关物质,所述检测方法操作简便、分离度高、测定方法专属性强、检测结果准确可信。
Description
技术领域
本发明设计药物检测技术领域,尤其涉及一种地红霉素原料有关物质的检测方法。
背景技术
地红霉素为大环内酯类抗生素,为红霉胺的前体药物,其作用机理是通过与敏感微生物的50S核糖体亚基结合,从而抑制细菌蛋白质合成。地红霉素部分在肝脏中代谢。大环内酯类抗生素都通过细胞色素P450微粒体酶系统产生去甲基化作用。地红霉素的代谢产物erythromycylamine具有相同的活性。本品主要由粪便与胆汁排泄,只有少量成分经尿排泄。代谢物随着服用方法的不同而不同。在其制取过程中会涉及多种原料物质,但是当前的检测方法操作复杂、分离度低、检测结果准确性低。
发明内容
为克服现有技术,本发明旨在于提供一种地红霉素原料有关物质的检测方法。
本发明是通过下面的技术方案实现,一种地红霉素原料有关物质的检测方法,该方法是采用高效液相色谱法进行的,包括下述步骤:
(1)配制地红霉素样品溶液,所述地红霉素样品溶液包括系统适用性溶液、供试品溶液、对照品溶液和灵敏度溶液;
(2)将步骤(1)所得样品溶液注入高效液相色谱仪,用流动相进行洗脱,并记录色谱图;其中,所述供试品溶液的制备方法包括下述步骤:精密称取地红霉素原料,加稀释液溶解并稀释至地红霉素的浓度为10mg/ml,得到供试品溶液;所述高效液相色谱法的色谱柱固定相填充剂为十八烷基硅烷键合硅胶;流动相的配制为水:甲醇:乙腈:磷酸盐缓冲溶液=14:19:39 :28。
优选的,所述磷酸盐缓冲溶液为取磷酸二氢钾1.9g与磷酸氢二钾9.1g,加水1000ml使溶解,并用100g/L氢氧化钾溶液调节PH至7.5。
优选的,所述高效液相色谱法的色谱条件,柱温为40℃,检测波长为205nm。
优选的,所述地红霉素样品溶液还包括系统适用性溶液、自身对照溶液和灵敏度溶液;
所述系统适用性溶液的制备方法包括下述步骤:取地红霉素对照品适量,加流动相溶解并稀释制成每1ml中含有2.5mg的溶液,室温放置至少24小时,作为系统适用性溶液;
所述自身对照溶液的制备方法包括下述步骤:精密量取供试品溶液1ml,置100ml 容量瓶中,加稀释液稀释至刻度,摇匀,得到自身对照溶液;
所述灵敏度溶液的制备方法包括下述步骤:精密量取对照品溶液1ml,置10ml 容量瓶中,加稀释液稀释至刻度,摇匀,得到地红霉素灵敏度溶液。
优选的,所述地红霉素供试品溶液中地红霉素的浓度为10mg/ml。
优选的,所述高效液相色谱法检测步骤(2)中,首先将样品灵敏度溶液注入液相色谱仪,调节检测器灵敏度,使主成分色谱峰的峰高为记录仪满量程的20%;再将系统适用性溶液、对照品溶液、供试品溶液分别注入液相色谱仪,采用流动相进行等度洗脱,并记录色谱图,注入液相色谱仪中样品溶液的量均为10μl。
本发明的检测方法在同一液相条件下测定地红霉素原料中的有关物质,所述检测方法操作简便、分离度高、测定方法专属性强、检测结果准确可信。
实施方式
实施例1
该方法是采用高效液相色谱法进行的,具体步骤如下:
(1)配制地红霉素样品溶液,所述地红霉素样品溶液包括系统适用性溶液、供试品溶液、对照品溶液和灵敏度溶液,地红霉素供试品溶液中地红霉素的浓度为10mg/ml。
(2)将步骤(1)所得样品溶液注入高效液相色谱仪,调节检测器灵敏度,使主成分色谱峰的峰高为记录仪满量程的20% ;再将系统适用性溶液、对照品溶液、供试品溶液分别注入液相色谱仪,用流动相进行洗脱,并记录色谱图,注入液相色谱仪中样品溶液的量均为10μl;其中,所述供试品溶液的制备方法包括下述步骤:精密称取地红霉素原料,加稀释液溶解并稀释至地红霉素的浓度为10mg/ml,稀释液由甲醇:乙腈=3:7配制,得到供试品溶液;所述高效液相色谱法的色谱柱固定相填充剂为十八烷基硅烷键合硅胶,所述色谱柱为XTerraRP18 4.6mm*250mm,3.5微米,柱温为40℃, 检测波长为205nm。流动相的配制为水:甲醇:乙腈:磷酸盐缓冲溶液=14:19 :39 :28,所述磷酸盐缓冲溶液为取磷酸二氢钾1.9g与磷酸氢二钾9.1g,加水1000ml使溶解,并用100g/L氢氧化钾溶液调节PH至7.5。
所述地红霉素样品溶液还包括系统适用性溶液、自身对照溶液和灵敏度溶液;
所述系统适用性溶液的制备方法包括下述步骤:取地红霉素对照品适量,加流动相溶解并稀释制成每1ml中含有2.5mg的溶液,室温放置至少24小时,作为系统适用性溶液。
所述自身对照溶液的制备方法包括下述步骤:精密量取供试品溶液1ml,置100ml容量瓶中,加稀释液稀释至刻度,摇匀,得到自身对照溶液;
所述灵敏度溶液的制备方法包括下述步骤:精密量取对照品溶液1ml,置10ml 容量瓶中,加稀释液稀释至刻度,摇匀,得到地红霉素灵敏度溶液。
Claims (6)
1.一种地红霉素原料有关物质的检测方法,该方法是采用高效液相色谱法进行的,其特征在于,包括下述步骤:
(1)配制地红霉素样品溶液,所述地红霉素样品溶液包括系统适用性溶液、供试品溶液、对照品溶液和灵敏度溶液;
(2)将步骤(1)所得样品溶液注入高效液相色谱仪,用流动相进行洗脱,并记录色谱图;其中,所述供试品溶液的制备方法包括下述步骤:精密称取地红霉素原料,加稀释液溶解并稀释至地红霉素的浓度为10mg/ml,得到供试品溶液;所述高效液相色谱法的色谱柱固定相填充剂为十八烷基硅烷键合硅胶;流动相的配制为水:甲醇:乙腈:磷酸盐缓冲溶液=14:19:39 :28。
2.根据权利要求1所述的检测方法,其特征在于,所述磷酸盐缓冲溶液为取磷酸二氢钾1.9g与磷酸氢二钾9.1g,加水1000ml使溶解,并用100g/L氢氧化钾溶液调节PH至7.5。
3.根据权利要求1所述的检测方法,其特征在于,所述高效液相色谱法的色谱条件,柱温为40℃,检测波长为205nm。
4.根据权利要求1所述的检测方法,其特征在于,所述地红霉素样品溶液还包括系统适用性溶液、自身对照溶液和灵敏度溶液;
所述系统适用性溶液的制备方法包括下述步骤:取地红霉素对照品适量,加流动相溶解并稀释制成每1ml中含有2.5mg的溶液,室温放置至少24小时,作为系统适用性溶液;
所述自身对照溶液的制备方法包括下述步骤:精密量取供试品溶液1ml,置100ml 容量瓶中,加稀释液稀释至刻度,摇匀,得到自身对照溶液;
所述灵敏度溶液的制备方法包括下述步骤:精密量取对照品溶液1ml,置10ml 容量瓶中,加稀释液稀释至刻度,摇匀,得到地红霉素灵敏度溶液。
5.根据权利要求1所述的检测方法,其特征在于,所述地红霉素供试品溶液中地红霉素的浓度为10mg/ml。
6.根据权利要求1所述的检测方法,其特征在于,所述高效液相色谱法检测步骤(2)中,首先将样品灵敏度溶液注入液相色谱仪,调节检测器灵敏度,使主成分色谱峰的峰高为记录仪满量程的20%;再将系统适用性溶液、对照品溶液、供试品溶液分别注入液相色谱仪,采用流动相进行等度洗脱,并记录色谱图,注入液相色谱仪中样品溶液的量均为10μl。
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Cited By (2)
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CN111060606A (zh) * | 2018-09-29 | 2020-04-24 | 湖南九典制药股份有限公司 | 一种地红霉素有关物质的检测方法 |
CN112697900A (zh) * | 2020-12-07 | 2021-04-23 | 澳美制药(苏州)有限公司 | 红霉素类抗生素干混悬剂的溶出度检测方法 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111060606A (zh) * | 2018-09-29 | 2020-04-24 | 湖南九典制药股份有限公司 | 一种地红霉素有关物质的检测方法 |
CN112697900A (zh) * | 2020-12-07 | 2021-04-23 | 澳美制药(苏州)有限公司 | 红霉素类抗生素干混悬剂的溶出度检测方法 |
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