肾上腺素原料药及盐酸肾上腺素注射液杂质的HPLC-QTOF MS分析

HPLC-QTOF MS analysis of impurities in epinephrine and epinephrine hydrochloride injection

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,1.8μm),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-[2-(丁基-2-基氨基)-1-羟乙基]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-[2-（butyl-2-ylamino）-1-hydroxyethyl]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.