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目的通过快速液相-四极杆飞行时间串联质谱(RRLC-QTOF)法分离、鉴定拉科酰胺粗品中4个未知杂质。方法采用美国Agilent RRLC快速液相色谱系统和6530型四极杆-飞行时间串联质谱仪,色谱柱为XDB-C18(150 mm×4.6 mm,5μm),流动相为醋酸铵-水溶液(甲酸调节pH至4.5)和乙腈,梯度洗脱,流速为1.0 mL·min-1,采用柱后分流,其中质谱仪进样流速为0.3 mL·min-1。结果结合高分辨质量数和二级质谱碎片推测得到了拉科酰胺粗品中4个可能的杂质结构。结论本研究为拉科酰胺的质量研究提供参考。
OBJECTIVE To isolate and identify four unknown impurities in the crude lactamide by rapid liquid chromatography-quadrupole time of flight tandem mass spectrometry (RRLC-QTOF). Methods The Agilent RLC LC system and the Model 6530 quadrupole-time of flight tandem mass spectrometer were used. The column was XDB-C18 (150 mm × 4.6 mm, 5 μm) and the mobile phase consisted of ammonium acetate-water solution To 4.5) and acetonitrile gradient elution. The flow rate was 1.0 mL · min-1. After the column was split, the mass flow rate was 0.3 mL · min-1. Results Based on the high resolution mass spectra and the second-order MS fragments, four possible impurity structures in the crude lactamide were obtained. Conclusion This study provides a reference for the quality of Lacosamide.