目的 建立HPLC测定富马酸伏诺拉生注射液中有关物质含量的方法.方法 采用YMC-Pack Pro C18 色谱柱(4.6mmX 150 mm,3 μm),流动相 A 为 0.04 mol·L-1 磷酸二氢钾溶液(含0.2％三乙胺,用磷酸调节pH至6.6)-乙腈-异丙醇(92∶4∶4),流动相B为0.04 mol·L-1磷酸二氢钾溶液(含0.2％三乙胺,用磷酸调节pH至6.6)-乙腈(40∶60),采用梯度洗脱,流速1.0mL·min-1,柱温40℃,检测波长220 nm,进样量20μL.结果 杂质H、杂质B、杂质C、杂质F、杂质D、杂质E、杂质J和伏诺拉生的质量浓度分别在0.12～4.99、0.12～4.99、0.12～4.90、0.13～5.01、0.12～4.99、0.13～5.01、0.13～5.01、0.13～5.01 μg·mL-1内与峰面积呈良好线性关系(r＞0.9990);7个杂质的回收率为94.72％～100.67％,其RSD值均小于2.0％;7个杂质和伏诺拉生的定量限为0.12～0.13μg·mL-1,检测限为0.040～0.043 μg·mL-1.结论 经方法学验证,本法专属性强、灵敏度高、准确度高,可用于富马酸伏诺拉生注射液中有关物质的含量测定.
HPLC determination of related substances in vonoprazan fumarate injection
Objective To establish an HPLC method to determine the related substances in vonoprazan fumarate injection.Methods YMC-Pack Pro C18 column(4.6 mm× 150 mm,3 μm)was used.Mobile phase A was 0.04 mol·L-1 potassium dihydrogen phosphate solution(containing 0.2％triethylamine,adjusted to pH 6.6 with phosphoric acid)-acetonitrile-isopropanol(92∶4∶4),while mobile phase B was 0.04 mol·L-1 potassium dihydrogen phosphate solution(containing 0.2％triethylamine,adjusted to pH 6.6 with phosphoric acid)-acetonitrile(40∶60).Gradient elution was used,the flow rate was 1.0 mL·min-1,the column temperature was 40 ℃,the detection wavelength was 220 nm,and the injection volume was 20 μL.Results Impurity H,impurity B,impurity C,impurity F,impurity D,impurity E,impurity J and vonoprazan all showed good linear relationship with the peak area at the concentration ranges of 0.12～4.99,0.12～4.99,0.12～4.90,0.13～5.01,0.12～4.99,0.13～5.01,0.13～5.01 and 0.13～5.01 μg·mL-1(r＞0.9990).The average recoveries of the above 7 impurities ranged 94.72％～100.67％,with all the RSD less than 2.0％.The quantitation limits of 7 impurities and vonoprazan were 0.12～0.13 μ·g·mL-1 and the detection limits were 0.040～0.043 μg·mL-1.Conclusion The method is exclusive,sensitive and accurate,which can be used to determine the related substances in vonoprazan fumarate injection.
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