CN113640418A - 盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法 - Google Patents
盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法 Download PDFInfo
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- GTNDZRUWKHDICY-DJHAJVGHSA-N Clindamycin palmitate hydrochloride Chemical compound Cl.O1[C@H](SC)[C@H](OC(=O)CCCCCCCCCCCCCCC)[C@@H](O)[C@@H](O)[C@H]1[C@@H]([C@H](C)Cl)NC(=O)[C@H]1N(C)C[C@H](CCC)C1 GTNDZRUWKHDICY-DJHAJVGHSA-N 0.000 title claims abstract description 59
- 229960000792 clindamycin palmitate hydrochloride Drugs 0.000 title claims abstract description 59
- 239000003814 drug Substances 0.000 title claims abstract description 39
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- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical group N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 10
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 10
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 10
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims abstract description 10
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 8
- 230000014759 maintenance of location Effects 0.000 claims abstract description 7
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- 239000012088 reference solution Substances 0.000 claims description 11
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- 229960001200 clindamycin hydrochloride Drugs 0.000 claims description 5
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Abstract
本发明公开了一种盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,采用高效液相色谱法进行检测,所述高效液相色谱法的固定相为十八烷基硅烷键合硅胶,流动相为醋酸铵溶液‑0.21%丁二酸二辛酯磺酸钠甲醇溶液;本发明提供的一种盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,在盐酸克林霉素棕榈酸酯特征峰2倍的保留时间内,即可检测出盐酸克林霉素棕榈酸酯原料药中的有关物质,检测时间短,而且本发明的方法可以采用等度洗脱,因此检测过程更加简便。
Description
技术领域
本发明涉及药品质量控制领域,特别涉及盐酸克林霉素棕榈酸酯中有关物质的检测方法。
背景技术
盐酸克林霉素棕榈酸酯(clindamycin palmitate hydochloride,CPH)是克林霉素的衍生物,它是一种新型林可霉素类抗生素,是克林霉素和棕榈酸酯化物的水溶性盐酸盐。
盐酸克林霉素棕榈酸酯在体外无活性,在体内能迅速转化为具有抗菌活性的克林霉素,具有较高的抗菌作用,对革兰阳性需氧菌、厌氧杆菌、衣原体、支原体均有活性。临床上广泛用于敏感菌引起的败血症、细菌性内膜炎、呼吸道、软组织、骨关节、耳部、泌尿生殖系统感染的治疗。
在盐酸克林霉素棕榈酸酯的合成过程以及后续的贮藏、运输、使用过程中,可能会产生一些与盐酸克林霉素棕榈酸酯结构相类似的有关物质(related substances),有关物质对于药物的疗效甚至安全性都可能会产生影响,因此,对于药品的质量控制而言,有关物质的检测是必不可少的。
发明内容
有鉴于此,本发明提供了一种盐酸克林霉素棕榈酸酯中有关物质的检测方法。
具体技术方案如下:
本发明提供了一种盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,采用高效液相色谱法进行检测,所述高效液相色谱法的固定相为十八烷基硅烷键合硅胶,流动相为醋酸铵溶液-0.21%丁二酸二辛酯磺酸钠甲醇溶液;
所述方法包括以下步骤:
(1)配制溶液:
将盐酸克林霉素棕榈酸酯原料药溶解后得到供试品溶液,然后取供试品溶液进行稀释,从而获得对照溶液;
(2)调节液相色谱仪:
取对照溶液注入液相色谱仪,调节检测灵敏度,使主成份盐酸克林霉素棕榈酸酯峰高为记录仪满程量的20%~25%;
(3)检测有关物质:
分别量取供试品溶液和对照溶液注入液相色谱仪,记录各自的色谱图至盐酸克林霉素棕榈酸酯特征峰保留时间的2倍;
将供试品溶液的色谱图和对照溶液的色谱图进行比较,从而确定盐酸克林霉素棕榈酸酯原料药中有关物质的含量。
在本发明的一些实施方式中,醋酸铵溶液和0.21%丁二酸二辛酯磺酸钠甲醇溶液的体积比为(15-25):(475-485)。
在本发明的一些实施方式中,醋酸铵溶液和0.21%丁二酸二辛酯磺酸钠甲醇溶液的体积比为20:480。
在本发明的一些实施方式中,所述高效液相色谱法采用等度洗脱。
在本发明的一些实施方式中,在供试品溶液的色谱图中显示杂质峰的情况下,将供试品溶液的色谱图中各杂质峰面积的总和与对照溶液的色谱图中的盐酸克林霉素棕榈酸酯特征峰的峰面积进行比较,根据二者的比值确定盐酸克林霉素棕榈酸酯原料药中有关物质的含量。
在本发明的一些实施方式中,步骤(1)中,采用流动相配制供试品溶液,并稀释供试品溶液。
在本发明的一些实施方式中,所述供试品溶液中盐酸克林霉素棕榈酸酯原料药的浓度为20mg/ml。
在本发明的一些实施方式中,所述对照溶液中盐酸克林霉素棕榈酸酯原料药的浓度为1mg/ml。
有益效果
本发明提供了一种盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,在盐酸克林霉素棕榈酸酯特征峰2倍的保留时间内,即可检测出盐酸克林霉素棕榈酸酯原料药中的有关物质,检测时间短,而且本发明的方法可以采用等度洗脱,因此检测过程更加简便。
附图说明
图1是实施例1中供试品溶液的高效液相色谱图;
图2是实施例1中对照溶液的高效液相色谱图。
具体实施方式
为使本申请的目的、技术方案和优点更加清楚,下面通过具体实施例将对本申请的技术方案进行清楚、完整地描述。
需要说明的是,以下实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
实施例1盐酸克林霉素棕榈酸酯原料药中有关物质的检测
检测对象:
内部批号为0801盐酸克林霉素棕榈酸酯原料药。
色谱条件:
仪器:岛津LC-9A高效液相色谱仪;岛津RID-10A示差折光检测器;JS-3050色谱工作站。
色谱柱:HYPERSIL ODS2(4.6mm×200mm,5μm)。
流动相:醋酸铵溶液-0.21%丁二酸二辛酯磺酸钠甲醇溶液(20∶480)
流速:1.0ml/min。
进样量:20μl。
检测步骤如下:
(1)配制溶液:
将盐酸克林霉素棕榈酸酯原料药加流动相溶解后得到20mg/ml的供试品溶液,然后取供试品溶液用流动相进行稀释,从而获得1.4mg/ml对照溶液;
(2)调节液相色谱仪:
取对照溶液20μl注入液相色谱仪,调节检测灵敏度,使主成份盐酸克林霉素棕榈酸酯峰高为记录仪满程量的20%~25%;
(3)检测有关物质:
分别量取供试品溶液和对照溶液20μl注入液相色谱仪,记录各自的色谱图至盐酸克林霉素棕榈酸酯特征峰保留时间的2倍,供试品溶液和对照溶液的色谱图分别如图1和图2所示;
将供试品溶液的色谱图和对照溶液的色谱图进行比较,在供试品溶液的色谱图中显示杂质峰的情况下,将供试品溶液的色谱图中各杂质峰面积的总和与对照溶液的色谱图中的盐酸克林霉素棕榈酸酯特征峰的峰面积进行比较,根据二者的比值确定盐酸克林霉素棕榈酸酯原料药中有关物质的含量,检测结果见表1。
实施例2盐酸克林霉素棕榈酸酯原料药中有关物质的检测
检测对象:
内部批号为0802盐酸克林霉素棕榈酸酯原料药。
色谱条件:
仪器:岛津LC-9A高效液相色谱仪;岛津RID-10A示差折光检测器;JS-3050色谱工作站。
色谱柱:HYPERSIL ODS2(4.6mm×200mm,5μm)。
流动相:醋酸铵溶液-0.21%丁二酸二辛酯磺酸钠甲醇溶液(15∶485)
流速:1.0ml/min。
进样量:20μl。
检测步骤如下:
(1)配制溶液:
将盐酸克林霉素棕榈酸酯原料药加流动相溶解后得到20mg/ml的供试品溶液,然后取供试品溶液用流动相进行稀释,从而获得1.4mg/ml对照溶液;
(2)调节液相色谱仪:
取对照溶液20μl注入液相色谱仪,调节检测灵敏度,使主成份盐酸克林霉素棕榈酸酯峰高为记录仪满程量的20%~25%;
(3)检测有关物质:
分别量取供试品溶液和对照溶液20μl注入液相色谱仪,记录各自的色谱图至盐酸克林霉素棕榈酸酯特征峰保留时间的2倍,供试品溶液和对照溶液的色谱图;
将供试品溶液的色谱图和对照溶液的色谱图进行比较,在供试品溶液的色谱图中显示杂质峰的情况下,将供试品溶液的色谱图中各杂质峰面积的总和与对照溶液的色谱图中的盐酸克林霉素棕榈酸酯特征峰的峰面积进行比较,根据二者的比值确定盐酸克林霉素棕榈酸酯原料药中有关物质的含量,检测结果见表1。
实施例3盐酸克林霉素棕榈酸酯原料药中有关物质的检测
检测对象
内部批号为0803盐酸克林霉素棕榈酸酯原料药。
色谱条件
仪器:岛津LC-9A高效液相色谱仪;岛津RID-10A示差折光检测器;JS-3050色谱工作站。
色谱柱:HYPERSIL ODS2(4.6mm×200mm,5μm)。
流动相:醋酸铵溶液-0.21%丁二酸二辛酯磺酸钠甲醇溶液(25∶475)
流速:1.0ml/min。
进样量:20μl。
检测步骤如下:
(1)配制溶液:
将盐酸克林霉素棕榈酸酯原料药加流动相溶解后得到20mg/ml的供试品溶液,然后取供试品溶液用流动相进行稀释,从而获得1.4mg/ml对照溶液;
(2)调节液相色谱仪:
取对照溶液20μl注入液相色谱仪,调节检测灵敏度,使主成份盐酸克林霉素棕榈酸酯峰高为记录仪满程量的20%~25%;
(3)检测有关物质:
分别量取供试品溶液和对照溶液20μl注入液相色谱仪,记录各自的色谱图至盐酸克林霉素棕榈酸酯特征峰保留时间的2倍,供试品溶液和对照溶液的色谱图;
将供试品溶液的色谱图和对照溶液的色谱图进行比较,在供试品溶液的色谱图中显示杂质峰的情况下,将供试品溶液的色谱图中各杂质峰面积的总和与对照溶液的色谱图中的盐酸克林霉素棕榈酸酯特征峰的峰面积进行比较,根据二者的比值确定盐酸克林霉素棕榈酸酯原料药中有关物质的含量,检测结果见表1。
表1
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域中的技术人员来说,本申请可以有各种修改和变化。凡在本申请的主旨和原则之内所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。
Claims (8)
1.一种盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,特征在于,采用高效液相色谱法进行检测,所述高效液相色谱法的固定相为十八烷基硅烷键合硅胶,流动相为醋酸铵溶液-0.21%丁二酸二辛酯磺酸钠甲醇溶液;
所述方法包括以下步骤:
(1)配制溶液:
将盐酸克林霉素棕榈酸酯原料药溶解后得到供试品溶液,然后取供试品溶液进行稀释,从而获得对照溶液;
(2)调节液相色谱仪:
取对照溶液注入液相色谱仪,调节检测灵敏度,使主成份盐酸克林霉素棕榈酸酯峰高为记录仪满程量的20%~25%;
(3)检测有关物质:
分别量取供试品溶液和对照溶液注入液相色谱仪,记录各自的色谱图至盐酸克林霉素棕榈酸酯特征峰保留时间的2倍;
将供试品溶液的色谱图和对照溶液的色谱图进行比较,从而确定盐酸克林霉素棕榈酸酯原料药中有关物质的含量。
2.根据权利要求1所述的盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,其特征在于,醋酸铵溶液和0.21%丁二酸二辛酯磺酸钠甲醇溶液的体积比为(15-25):(475-485)。
3.根据权利要求2所述的盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,其特征在于,醋酸铵溶液和0.21%丁二酸二辛酯磺酸钠甲醇溶液的体积比为20:480。
4.根据权利要求2所述的盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,其特征在于,所述高效液相色谱法采用等度洗脱。
5.根据权利要求1所述的盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,其特征在于,在供试品溶液的色谱图中显示杂质峰的情况下,将供试品溶液的色谱图中各杂质峰面积的总和与对照溶液的色谱图中的盐酸克林霉素棕榈酸酯特征峰的峰面积进行比较,根据二者的比值确定盐酸克林霉素棕榈酸酯原料药中有关物质的含量。
6.根据权利要求1所述的盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,其特征在于,步骤(1)中,采用流动相配制供试品溶液,并稀释供试品溶液。
7.根据权利要求1所述的盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,其特征在于,所述供试品溶液中盐酸克林霉素棕榈酸酯原料药的浓度为20mg/ml。
8.根据权利要求1所述的盐酸克林霉素棕榈酸酯原料药中有关物质的检测方法,其特征在于,所述对照溶液中盐酸克林霉素棕榈酸酯原料药的浓度为1mg/ml。
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