正相高效液相色谱法测定枸橼酸托法替尼原料及片剂中对映异构体

发布时间：2019-06-29 11:03

【摘要】：目的:建立枸橼酸托法替尼原料及片剂中对映异构体含量的测定方法。方法:采用正相高效液相色谱法测定。色谱条件:以手性柱Chiralpak AD-H(250 mm×4.6 mm,5μm)为色谱柱;以正己烷-异丙醇-甲醇(71∶21∶8)-三乙胺(100∶0.2)溶液为流动相;检测波长:280 nm;流速:0.5 mL·min~(-1);柱温:30℃;进样量:5μL。结果:该方法专属性良好,片剂中辅料无干扰,对映异构体与相邻峰的分离度均大于2.0;精密度(RSD=0.0%,n=6)和中间精密度(RSD=5.9%,n=12)良好;加样回收率为91.2%~96.4%(RSD=3.0%,n=9);检测限和定量限分别为0.08μg·mL~(-1)和0.16μg·mL~(-1),分别约为供试品溶液浓度的0.02%和0.04%;线性范围为0.16~8.00μg·mL~(-1)(r=1.000);供试品溶液至少在34 h内稳定;3批原料样品中对映异构体含量分别为:0.01%、0.02%、0.04%;3批制剂(片剂)样品中对映异构体含量分别为:0.01%、0.02%、0.05%。结论:本法经方法学验证,可用于测定枸橼酸托法替尼原料及片剂中对映异构体杂质的含量。
[Abstract]:Objective: to establish a method for the determination of enantiomers in torfatinib citrate raw materials and tablets. Methods: the method was determined by normal phase high performance liquid chromatography (HPLC). The chromatographic conditions were as follows: chiral column Chiralpak AD-H (250 mm 脳 4.6 mm, 5 渭 m), n-hexane-isopropanol-methanol (71:21:8)-triethylamine (100 鈮，

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