二丙酸倍他米松有关物质的HPLC法测定
Determination of related substances in betamethasone dipropionate by HPLC
唐玲玲 1葛纪龙 2陶永新3
作者信息
- 1. 常州大学石油化工学院,江苏 常州 213164;常州四药制药有限公司,江苏 常州 213018
- 2. 常州四药制药有限公司,江苏 常州 213018
- 3. 常州大学石油化工学院,江苏 常州 213164
- 折叠
摘要
建立了高效液相色谱法测定二丙酸倍他米松(1)中的有关物质,即倍他米松(2)、倍他米松17-丙酸酯(3)、二丙酸倍氯米松(4)、6α-溴倍他米松二丙酸酯(5).色谱柱选用COSMOSIL 5C18-MS-Ⅱ(4.6mm×150mm,5 μm),以0.04％三氟乙酸-H2O为流动相A、0.02％三氟乙酸-乙腈为流动相B,梯度洗脱;流速为 0.8 mL/min,检测波长为 254 nm,柱温40℃.结果显示,1 和杂质 2～5 均分离良好,且在各自浓度范围内线性关系良好;2～5 的平均回收率(n=9)为 99.8％～104.2％,RSD为 4.0％～6.1％.1、2、4 的检测限为 0.1 μg/mL,3 和5 的检测限为0.2 μg/mL.建立的方法准确性好、灵敏度高,各组分分离较好,可用于 1 中有关物质的测定.
Abstract
An HPLC method is established for the determination of the related substances such as betamethasone,betamethasone-17-propionate,beclomethasone dipropionate and 6-α-bromo-betamethasone dipropionate in betamethasone dipropionate.COSMOSIL 5C18-MS-Ⅱ column(4.6 mm×150 mm,5 μm)is used in the gradient elution mode,with 0.04%trifluoroacetic acid-H2O as mobile phase A and 0.02%trifluoroacetic acid-acetonitrile as mobile phase B.The flow rate is 0.8 mL·min-1,the wavelength used for detection is 254 nm,and the column temperature is maintained at 40℃.It is shown by the result that betamethasone dipropionate is separated well with the related four substances,and the peaks of the related substances show linear in their corresponding concentration ranges.The average recoveries(n=9)of betamethasone,betamethasone-17-propionate,beclomethasone dipropionate and 6-α-bromo-betamethasone dipropionate are in the range of 99.8%-104.2%,with RSDs of 4.0%-6.1%.The detection limits are 0.1 μg·mL-1 for betamethasone dipropionate,betamethasone and beclomethasone dipropionate,and 0.2 μg·mL-1 for betamethasone-17-propionate and 6-α-bromo-betamethasone dipropionate.The established method has good accuracy and high sensitivity as well as good separation effect for each component,which can be used for the determination of the related substances in betamethasone dipropionate.
关键词
二丙酸倍他米松/有关物质/高效液相色谱Key words
betamethasone dipropionate/related substance/HPLC引用本文复制引用
出版年
2024
NETL
NSTL
万方数据