摘要
目的建立高效液相色谱法测定利托那韦起始物料N-〔N-甲基-N-〔(2-异丙基-4-噻唑基)甲基〕氨基羰基〕-L-缬氨酸的有关物质含量。方法采用Agilent Poroshell 120 Phenyl-Hexyl(100 mm×4.6 mm,2.7μm)色谱柱;流动相A为水-乙腈-三氟乙酸(90∶10∶0.1),流动相B为乙腈-甲醇-三氟乙酸(50∶50∶0.1);柱温35℃;梯度洗脱,流速1.0 mL·min^(-1),检测波长220 nm。结果利托那韦起始物料及其各有关物质在各自线性范围内呈良好的线性关系(r≥0.990);各有关物质加样回收率在86.7%~115.1%之间,RSD(n=9)≤8.5;系统适用性溶液中,主成分及各有关物质与邻近色谱峰之间分离度均大于1.5。结论该方法灵敏度高、专属性强、准确度高,适用于利托那韦起始物料有关物质的检测。
OBJECTIVE To establish an efficient liquid chromatography method for the determination of related substances in N-〔N-methyl-N-〔(2-isopropyl-4-thiazolyl)methyl amino〕carbonyl〕-L-valine.METHODS A gradient elution was performed on an Agilent Poroshell 120 Phenyl-Hexyl(100 mm×4.6 mm,2.7μm)column with water-acetylene-trifluorocetic acid[JP3](90∶10∶0.1)as mobile phase A,and acetylene-methanol-trifluorocetic acid(50∶50∶0.1)[JP]as mobile phase B at a flow rate of 1.0 mL·min^(-1).The detection wavelength was 220 nm,the column temperature was 35℃.RESULTS Ritonavir starting material and its impurities showed good linear relationship(r≥0.990);The average recoveries of impurities were within 86.7%-115.1%,and the RSD(n=9)of the recovery rate was less than 8.5;The separation degree between the peaks of related substances and the principal peak obtained in chromatogram of the system suitability solution were greater than 1.5.CONCLUSION The detection method has high sensitivity,strong specificity,and high accuracy.It could be used for the determination of related substances of ritonavir starting material.
作者
胡中志
梅青
郭宾
罗江胜
HU Zhong-zhi;MEI Qing;GUO bin;LUO Jiang-sheng(Wuhan Haite Biological Innovation Pharmaceutical Research Co.,Ltd.,Wuhan 430073,China)
出处
《海峡药学》
2024年第10期32-36,共5页
Strait Pharmaceutical Journal
关键词
高效液相色谱法
利托那韦起始物料
有关物质
质量控制
High performance liquid chromatography
Ritonavir starting material
Related Substances
Quality control
