高效液相色谱法测定非那雄胺中5β-非那雄胺
Determination of 5β-finasteride in Finasteride by HPLC
蒋晨 1李金鹏 2丁晓晓 1张浩 1王琛1
作者信息
- 1. 南京圣和药业股份有限公司,江苏 南京 210000
- 2. 南京圣和药业股份有限公司,江苏 南京 210000;中国药科大学,江苏 南京 210009
- 折叠
摘要
目的:建立高效液相色谱方法用于测定非那雄胺原料药中的 5β-非那雄胺.方法:采用Welch Xtimate C18(4.6×150 mm,3.5 μm)色谱柱,以8%的四氢呋喃水溶液为流动相A,以 8%的四氢呋喃乙腈溶液为流动相B,梯度洗脱,流速为 1.0 mL/min,检测波长为 210 nm,柱温25℃,对非那雄胺原料药中的5β-非那雄胺进行定量分析.结果:该液相色谱方法中5β-非那雄胺与非那雄胺及相邻杂质分离良好,且非那雄胺原料药在各强制破坏条件下均未产生干扰5β-非那雄胺的杂质,方法专属性良好;5β-非那雄胺与非那雄胺分别在0.27～2.17和0.28～2.23 μg·mL-1浓度范围内线性良好(r≥0.990);5β-非那雄胺的加样回收率为108.2%;进样精密度和重复性良好;系统适用性溶液和供试品溶液室温条件放置94小时和 82小时稳定;各耐用性条件下 5β-非那雄胺与非那雄胺的分离度均在 4.10～4.80之间,方法耐用性良好.结论:本文所建立的分析方法专属性好、准确度高,简便耐用,可用于非那雄胺原料药中5β-非那雄胺的定量分析.
Abstract
Objective:To establish a HPLC method for the determination of 5β-finasteride in finasteride.Method:The separation was achieved on Welch Xtimate C18(4.6×150 mm,3.5 μm)column using 8%tetrahydrofuran in water(mobile phase A)and 8%tetrahydrofuran in acetonitrile(mobile phase B)with gradient elution program.The flow rate was kept at 1.0 mL/min at 25℃,the detection wavelength was 210 nm.Results:In this method,the well separation of 5β-finasteride from finasteride,impurities(A,B,C and 17α-finasteride)and the other impurities produced from the forced degradation tests of finasteride which proved the method was specific.The results showed a good linear relationship(r≥0.990)between the concentrations of 5β-finasteride and finasteride in the ranges of 0.27～2.17 and 0.28～2.23 μg·mL-1,respectively.The recovery of 5β-finasteride was 108.2%.The injection precision and repeatability were good.The resolution solution and the sample solution were stable for 94 hours and 82 hours at room temperature.The resolutions between 5β-finasteride and finasteride were 4.10～4.80 under different chromatograph conditions with good durability.Conclusion:The method was established with good specificity,high accuracy,simple and durable which can be used for the quantitative analysis of 5β-finasteride in finasteride.
关键词
5β-非那雄胺/雄性激素脱发/高效液相色谱法/非那雄胺/方法学验证Key words
5β-finasteride/androgenetic alopecia/HPLC/finasteride/methodology validation引用本文复制引用
出版年
2024
NETL
NSTL
万方数据