液相色谱-质谱联用技术鉴定甘草酸二铵肠溶片中有关物质

Determination of related substances in Diammonium Glycyrrhizinate Enteric Coated Tablet by LC-MS

目的建立超高效液相-二极管阵列-离子阱-飞行时间串联质谱（UPLC-DAD-IT-TOF-MS）法分离鉴定甘草酸二铵肠溶片中相关杂质的分析方法。方法采用Agilent HC-C18（250 mm×4.6 mm,5μm）色谱柱,以乙腈-水-冰醋酸（380∶614∶6）为流动相等度洗脱样品,体积流量1 m L/min,紫外检测波长254 nm,质谱监测质荷比范围m/z 100~1 000。结果分离鉴定出甘草酸皂苷G2、H2、E2、B2、J2、C2及18α-甘草酸、乌拉尔甘草皂苷（A或B）8种有关物质。结论研究结果为甘草酸二铵肠溶片的质量控制和工艺优化提供了依据,同时为中药制剂的杂质鉴定提供可借鉴的分析思路。

Objective To establish the methods for identifying the related substances in Diammonium Glycyrrhizinate Enteric Coated Tablet （DGECT） by ultra high performance liquid-diode array-ion trap-the time of flight tandem mass spectrometry （UPLC-DAD-IT- TOF-MS）. Methods The chromatographic separation was performed on an Agilent HC-C18 （250 mm × 4.6 mm, 5 μm） column, mobile phase was acetonitril-H20-Hac （380 ： 614 ： 6）, eluting sample was in equal degree flow, with volume flow rate of 1 mL/min, UV detection wavelength of 254 nm, and mass spectrum monitoring mass-to-charge ratio range m/z 100-1 000. Results Including licoricesaponine G2, H2, E2, B2, J2, C2, 18ct-glycyrrhizic acid, and glycyrrhiza uralensis saponin （A or B）, the eight kinds of related compounds existed were found. Conclusion The related substances found in DGECT are valuable for the manufacturing process and quality control.