UPLC-MS/MS法同时测定血必净注射液中15种有效成分的含量

Simultaneous determination of 15 components in Xuebijing injection by UPLC-MS/MS

关键词:  血必净注射液  超高效液相色谱-质谱联用  含量测定

Key words:  Xuebijing injection  UPLC-MS/MS  determination

摘要:

[目的]建立同时测定血必净注射液中15种有效成分含量的测定方法，并用于10批血必净注射液的含量测定。[方法]采用超高效液相色谱-质谱联用仪（UPLC-MS/MS），色谱柱为ACQUITY UPLC^®BEH C₁₈柱（2.1 mm×100 mm，1.7 μm），以乙腈、0.1%甲酸水为流动相进行梯度洗脱，洗脱时间为6 min，流速为0.3 mL/min，电喷雾离子源，多重反应监测（MRM）模式进行负离子扫描。[结果]各目标成分线性关系良好，方法学精密度RSD值为1.02%~4.94%，重复性RSD值为2.13%~4.99%，加样回收率为94.89%~105.34%，除没食子酸外各成分在12 h内均稳定。对10批不同批次血必净注射液含量测定结果表明，目标成分中芍药苷含量最高，原儿茶酸含量最低。[结论]该方法简便、快捷，可用于血必净注射液的质量控制。

Abstract:

[Objective] To develop an UPLC-MS/MS method for simultaneous determination of 15 components in Xuebijing injection from 10 different batchs.[Methods] UPLC-MS/MS was adopted. The separation was completed on an Waters ACQUITY UPLC^® C₁₈ (2.1 mm×100 mm, 1.7 μm) column using 0.1% (V/V) formic acid and actonitrile as mobile phase in gradient elution mode. The gradient elution time was in 6 minutes. The flow rate was set at 0.3 mL/min. The mass spectrometer was operated under the negative ion mode with the ESI source and MRM mode was used for quantification.[Results] All of the 15 components showed good linearity in the test ranges. The RSDs of precision were 1.02%~4.94%. The RSDs of reproducibility were 2.13%~4.99%. The recoveries of them were 94.89%~105.34%. All the components were stable in 12 h except gallic acid. The results showed that the content of paeoniflorin was the highest in the target group, and the content of protocatechuic acid was the lowest.[Conclusion] The method is simple, rapid and can be used for the quality control of 15 components in Xuebijing injection.