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建立了高效液相色谱法测定克唑替尼的含量和光学纯度。采用Shim-pack VP-ODS C18色谱柱对克唑替尼进行含量测定,以甲醇(含0.1%三氟乙酸)-水(含0.1%三氟乙酸)为流动相进行梯度洗脱;流速为0.6 m L/min;检测波长为268 nm;柱温为25℃。采用岛津CHIRALPAKAD-H色谱柱对克唑替尼进行光学纯度测定,以V(正己烷)∶V(异丙醇)∶V乙醇)∶V(二乙胺)=50∶25∶25∶0.2为流动相,流速为0.6 m L/min,检测波长为268 nm,柱温为30℃。结果表明,克唑替尼质量浓度在0.05~2.51 mg/m L范围内与峰面积呈良好的线性关系(r=0.999 9)。克唑替尼与其异构体杂质能完全分离。该方法简便、可靠,可用于克唑替尼的质量控制。
A high performance liquid chromatography was established for the determination of crizotinib content and optical purity. The content of crizotinib was determined by Shim-pack VP-ODS C18 column with gradient elution with methanol (containing 0.1% trifluoroacetic acid) -water (containing 0.1% trifluoroacetic acid) as the mobile phase. The flow rate was 0.6 m L / min; detection wavelength was 268 nm; column temperature was 25 ℃. The optical purity of crizotinib was determined by using Shimadzu CHIRALPAK AD-H column. V (n-hexane): V (isopropanol): V ethanol): V : 0.2 as the mobile phase at a flow rate of 0.6 m L / min with a detection wavelength of 268 nm and a column temperature of 30 ° C. The results showed that the concentration of crizotinib in the range of 0.05 ~ 2.51 mg / m L showed a good linear relationship with the peak area (r = 0.999 9). Crizotinib and its isomer impurities can be completely separated. The method is simple and reliable and can be used for the quality control of crizotinib.