肾上腺素原料药及盐酸肾上腺素注射液杂质的HPLC-QTOFMS分析

目的: 建立HPLC-QTOF MS法测定肾上腺素原料药及盐酸肾上腺素注射液杂质。 方法: 采用Eclipse plus C₁₈ 色谱柱(3.0 mm×100 mm,1.8 μm),以5 mmol·L^-1 甲酸铵水溶液-0.1%甲酸水溶液(A)/ 乙腈(B)为流动相,流速为0.3 mL·min^-1,梯度洗脱,梯度条件如下:0→4 min,2% B;4→10 min,2%~50% B;10→12 min,50%~90%B;12→15 min,90%B;柱温为30℃。采用正离子模式采集数据。 结果: 原料药和注射液中共检出3个杂质,分别为肾上腺酮、肾上腺素磺化物和4- 苯酚。 结论: 本法简便、灵敏,准确,可用于肾上腺素原料药及制剂的杂质定性分析。

Objective: To develop an HPLC-QTOF MS method for analysis of impurities in epinephrine and epinephrine hydrochloride injection. Methods: An Eclipse plus C₁₈ column(3.0 mm×100 mm,1.8 μm) was utilized.The mobile phase was 5 mmol·L^-1 ammonium formate aqueous solution (5 mmol·L^-1)-formic acid aqueous solution (0.1%) (A) or acetonitrile (B).The velocity was 0.3 mL·min^-1.The gradient elution was carried out in the following conditions:0→4 min,2% B;4→10 min,2%-50% B;10→12 min,50%-90%B;12→15 min,90%B.The column temperature was 30℃.The data was collected in positive ion mode. Results: Three impuries were found in epinephrine and epinephrine hydrochloride injection.They were adrenalone,sulfonated epinephrine and 4- phenol. Conclusion: The method is simple,sensitive and accurate.It can be used for the qualitative analysis of impurities in epinephrine and epinephrine hydrochloride injection.

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