手性HPLC法检查S-萘普生中R-异构体杂质

Determination of R-isomer Impurity in S-naproxen by Chiral HPLC

文章建立测定右旋萘普生(S-萘普生)中对映异构体杂质(R-萘普生)含量的手性高效液相色谱(HPLC)方法,采用Chiralpak ID(250 mm×4.6 mm,5µm)手性色谱柱,以20 mmol/L醋酸铵缓冲液(pH 3.5)-甲醇(体积比40∶60)为流动相,检测波长为230 nm,流速为0.6 mL/min,柱温为25℃。其实验结果表明,R-萘普生和S-萘普生在浓度为0.20~0.60µg/mL范围内线性关系良好(r=0.9996),检测限分别为0.04µg/mL和0.05µg/mL,定量限分别为0.12µg/mL和0.15µg/mL,方法回收率为95.0%~106.5%(RSD=4.5%,n=6)。该方法简单可靠、灵敏度高、专属性强,符合化学药物杂质检查的规定,适用于S-萘普生原料药中R-异构体杂质的检查。

A chiral high performance liquid chromatography(HPLC)method for the determination of enantiomer impurity(R-naproxen)in D-naproxen(S-naproxen)was established.Chiralpak ID(250 mm×4.6 mm,5μm)chiral chromatographic column was used.20 mmol/L ammonium acetate buffer(pH 3.5)-methanol(volume ratio 40∶60)was used as the mobile phase.The detection wavelength was 230 nm,the flow rate was 0.6 mL/min,and the column temperature was 25℃.The experimental results showed that the linear relationship between R-naproxen and S-naproxen was good(r=0.9996)in the concentration range of 0.20-0.60μg/mL,the detection limits were 0.04μg/mL and 0.05μg/mL,and the limits of quantification were 0.12μg/mL and 0.15μg/mL,respectively,the method recoveries were 95.0%-106.5%(RSD=4.5%,n=6).The method is simple,reliable,sensitive and specific,it is suitable for the inspection of R-isomer impurities in S-naproxen raw materials.