目的:建立一种UPLC-MS/MS法同时测定舒肝宁注射液中6个成分(绿原酸、栀子苷、黄芩苷、黄芩素、野黄芩苷、表告依春)的含量。方法:采用XBridge BEH C18色谱柱(2.1 mm×100 mm,2.5 μm),以乙腈(A)-0.05%甲酸水(B)溶液为流动相进行梯度洗脱(0~3 min,25% A→90% A;3~5 min,90% A→90% A),流速0.3 mL·min-1,进样量5 μL;柱温为30℃;采用电喷雾离子源进行正负离子同时监测,多反应监测模式(MRM)用于定量分析。结果:在5 min内,舒肝宁注射液的6个成分(绿原酸、栀子苷、黄芩苷、黄芩素、野黄芩苷、表告依春)被完全分离,峰面积与浓度有良好的线性关系,相关系数(r)均大于0.999 6。试验精密度、重复性和稳定性良好;平均加样回收率为95.1%~100.1%。5批样品中绿原酸、栀子苷、黄芩苷、黄芩素、野黄芩苷、表告依春含量测定结果分别为50.32~52.16、526.1~555.6、18 401~19 594、205.9~262.1、115.1~122.5、28.38~30.95 ng·mL-1。结论:本方法快速准确灵敏,重复性好,可用于舒肝宁注射液中6个成分的定量测定。
Objective: To develop a method for the simultaneous determination of the chlorogenic acid,geniposide,baicalin,baicalein,scutellarin and epigoitrin in Shuganning injection by UPLC-MS/MS. Methods: The samples were separated on an XBridge BEH C18 column(2.1 mm×100 mm,2.5 μm). The mobile phase composed of acetonitrile(A) and 0.05% aqueous formic acid(B) with gradient elution(0-3 min,25%A→90%A;3-5 min,90%A→90%A). The injection volume was 5 μL and the flow rate was 0.3 mL·min-1. The column temperature was 30℃. Multiple-reaction monitoring(MRM) scanning was employed for quantification with switching electrospray ion source polarity in positive and negative ions. Results: The six components in Shuganning injection(chlorogenic acid,geniposide,baicalin,baicalein,scutellarin,epigoitrin) were completely separated in 5 minutes. The regression equations showed linear relationships between the peak area and concentration of each component. The correlation coefficients(r) were above 0.999 6. The precision,repeatability,and stability of the method were good for all six components. The average recoveries ranged from 95.1% to 100.1%. The contents of chlorogenic acid,geniposide,baicalin,baicalein,scutellarin and epigoitrin in 5 batches of samples were 50.32-52.16,526.1-555.6,1 8401-19 594,205.9-262.1,115.1-122.5 and 28.38-30.95 ng·mL-1,respectively. Conclusion: The method is rapid,accurate and sensitive with good reproducibility and can be used for the determination of 6 compounds in Shuganning injection.