目的:采用主成分自身对照法测定注射用奥美拉唑钠中的7个已知杂质。方法:采用Waters XBridge C8色谱柱(250 mm×4.6 mm,5 μm),以磷酸盐缓冲液(pH 7.0)-乙腈为流动相,梯度洗脱,流速1.0 mL·min-1,柱温25 ℃,检测波长280 nm。采用加校正因子的主成分自身对照法计算7个已知杂质的含量。结果:在所选定的液相色谱条件下,主成分和7个已知杂质出峰顺序依次为杂质Ⅱ、杂质Ⅳ、杂质Ⅷ、杂质Ⅴ、奥美拉唑、杂质Ⅰ、杂质Ⅲ和杂质Ⅸ/Ⅹ,各峰间的分离度均符合规定,各杂质检测限依次为1.0、0.3、0.7、0.7、2.2、2.7和1.8 ng。3批次样品均检出了杂质Ⅲ和杂质Ⅳ,主成分自身对照法所得结果与外标法基本一致,2种方法测定的结果最多相差0.02%。结论:该方法操作简单,成本低,实用性强,专属性强,可用于注射用奥美拉唑钠的杂质检查。
Objective: To establish a RP-HPLC method for determination of seven impurities in omeprazole sodium for injection by main component self-compare method. Methods: The separation was performed on Waters XBridge C8 column (250 mm×4.6 mm, 5 μm) with gradient elution, Using phosphate buffer (pH 7.0)-acetonitrile as the mobile phase. The flow rate was 1.0 mL·min-1, the column temperature was 25 ℃, the detection wavelength was 280 nm. And relative correction factors were used to calculate the content of seven known impurities. Results: Under the selected liquid chromatographic conditions, the peak sequence of the principal component and the seven known impurities was impurites Ⅱ, Ⅳ, Ⅷ, Ⅴ, omeprazole, impurity Ⅰ, Ⅲ and Ⅸ/Ⅹ, the resolution between each peak was in line with the regulations, and the detection limits of each impurity were 1.0 ng, 0.3 ng, 0.7 ng, 0.7 ng, 2.2 ng, 2.7 ng and 1.8 ng, separately. Impurity Ⅲ and impurity Ⅳ were detected in all three batches of samples. The results obtained by main component self-compare method were no significant differentiation with those obtained by external standard method, and the difference between the two methods was 0.02% at most. Conclusion: The method has the advantages of simple operation, low cost, strong practicability and specificity, and could be used for the impurity inspection of omeprazole sodium for injection.
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