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目的建立伏立康唑冻干眼用制剂中有关物质的检查方法。方法采用RP-HPLC法,色谱柱为Thermo Hypersil GOLD C18(250 mm×4.6 mm,5μm);检测波长为256 nm;柱温为35℃;进样量为20μL;流速为1.0 m L·min-1,以甲醇-乙腈-水为流动相,梯度洗脱。结果伏立康唑及各杂质均能得到良好的分离。伏立康唑、杂质A、C和EPC在0.25~5.0 mg·L~(-1)内,杂质D在0.5~2.0 mg·L~(-1)内线性关系良好(r>0.999 0,n=6)。伏立康唑、杂质A、C和EPC质量浓度为2.5 mg·L~(-1),杂质D质量浓度为1.0 mg·L~(-1)时,精密度(RSD)分别为1.3%、1.6%、1.5%、1.3%和1.3%;杂质A、C、D和EPC平均回收率分别为101.2%、101.3%、96.6%和96.6%。经对供试品测定,除杂质D未检出外,其余杂质A、C和EPC峰面积RSD分别为0.02%、0.01%和1.2%。结论该方法适用于伏立康唑冻干眼用制剂的有关物质检查。
Objective To establish a method for the determination of related substances in voriconazole freeze-dried ophthalmic preparations. Methods The RP-HPLC method was used. The column was Thermo Hypersil GOLD C18 (250 mm × 4.6 mm, 5 μm), the detection wavelength was 256 nm, the column temperature was 35 ℃, the injection volume was 20 μL, the flow rate was 1.0 m L · min- 1, with methanol - acetonitrile - water as mobile phase, gradient elution. Results Voriconazole and various impurities can be a good separation. Voriconazole, impurity A, C and EPC were well linear within the range of 0.5 ~ 2.0 mg · L -1 with 0.25 ~ 5.0 mg · L -1 impurities (r> 0.999 0, n = 6) . The results showed that the precision (RSD) of voriconazole was 1.3% and 1.6% when the concentration of impurity A, C and EPC was 2.5 mg · L -1 and the concentration of impurity D was 1.0 mg · L -1, 1.5%, 1.3% and 1.3% respectively. The average recoveries of impurities A, C, D and EPC were 101.2%, 101.3%, 96.6% and 96.6%, respectively. The RSDs of the other impurities A, C and EPC were 0.02%, 0.01% and 1.2% respectively, except for the impurities D were not detected. Conclusion The method is suitable for voriconazole freeze-dried eye preparations related substances.