丁建营, 刘发贵, 王花, 刘思光, 李铁健, 张贵民. 超高效合相色谱法测定缬沙坦原料药中R-缬沙坦[J]. 分析测试技术与仪器, 2022, 28(4): 405-410. DOI: 10.16495/j.1006-3757.2022.04.006
引用本文: 丁建营, 刘发贵, 王花, 刘思光, 李铁健, 张贵民. 超高效合相色谱法测定缬沙坦原料药中R-缬沙坦[J]. 分析测试技术与仪器, 2022, 28(4): 405-410. DOI: 10.16495/j.1006-3757.2022.04.006
DING Jian-ying, LIU Fa-gui, WANG Hua, LIU Si-guang, LI Tie-jian, ZHANG Gui-min. Determination of R-valsartan in Valsartan Active Pharmaceutical Ingredients by Ultra Performance Convergence Chromatography[J]. Analysis and Testing Technology and Instruments, 2022, 28(4): 405-410. DOI: 10.16495/j.1006-3757.2022.04.006
Citation: DING Jian-ying, LIU Fa-gui, WANG Hua, LIU Si-guang, LI Tie-jian, ZHANG Gui-min. Determination of R-valsartan in Valsartan Active Pharmaceutical Ingredients by Ultra Performance Convergence Chromatography[J]. Analysis and Testing Technology and Instruments, 2022, 28(4): 405-410. DOI: 10.16495/j.1006-3757.2022.04.006

超高效合相色谱法测定缬沙坦原料药中R-缬沙坦

Determination of R-valsartan in Valsartan Active Pharmaceutical Ingredients by Ultra Performance Convergence Chromatography

  • 摘要: 建立了基于超高效合相色谱法(UPCC)分离和检测缬沙坦原料中对映异构体R-缬沙坦的分析方法,并探讨测定时主要影响因素. 采用多糖衍生的手性柱(CHIRALPAK IC-3, 100 mm×3.0 mm, 3 μm),以甲醇(含0.5%乙醇胺)∶二氧化碳(体积比为20∶80)为流动相,等度洗脱,流速为1 mL/min,检测波长为230 nm,动态背压(ABPR)13.79 MPa. 在10.072~100.720 μg/mL质量浓度范围内,可有效分离R-缬沙坦. 线性回归方程:Y=428.910 5X−1.059 8(r=0.998 0,n=7),检测限为3.357 μg/mL,平均回收率为104.35%(n=9). 试验结果表明,方法快速、高效、经济、环保,为缬沙坦原料中R-缬沙坦的测定提供了新的方法与思路.

     

    Abstract: An analytical method based on the ultra performance convergence chromatography (UPCC) has been established for the separation and detection of the enantiomer R-valsartan in valsartan raw materials, and the main influencing factors have been discussed. A polysaccharide-derived chiral column (CHIRALPAK IC-3, 100 mm×3.0 mm, 3 μm) was used with methanol (containing 0.5% ethanolamine)∶carbon dioxide as the mobile phase and an isocratic elution at a flow rate of 1 mL/min with a detection wavelength of 230 nm and a dynamic back pressure (ABPR) of 13.79 MPa. The R-valsartan was effectively isolated in the range of 10.072~100.720 μg/mL, the linear regression equation was Y=428.910 5X−1.059 8 (r=0.998 0, n=7), the detection limit was 3.357 μg/mL, and the average recovery rate was 104.35% (n=9). The detection and analysis method of R-valsartan by UPCC was established, which is fast, efficient, economical and environmentally friendly, and provides a new method and idea for the determination of R-valsartan in valsartan raw materials.

     

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