HPLC-MS法同时测定舒血宁注射液中萜类内酯和黄酮醇苷的含量

目的:建立HPLC-MS法同时测定舒血宁注射液中银杏内酯A(GA)、银杏内酯B(GB)、银杏内酯C(GC)、白果内酯(BB)以及槲皮素(QCT)、异鼠李素(ISR)和山柰酚(KAE)的含量。方法:采用Dikma Diamonsil C₁₈色谱柱(150 mm×4.6 mm, 5 μm), 柱温30℃, 以乙腈-0.05%甲酸水(v/v)溶液为流动相进行梯度洗脱, 流速0.8 mL·min^-1, 进样量10 μL;采用电喷雾离子源进行负离子模式监测, 多反应监测模式(MRM)用于定量分析, 源喷射电压为-4.5 kV, 离子源温度为650℃。7个被测成分的检测离子对分别为m/z 453.1/351.2(GA), m/z 423.1/367.0(GB), m/z 439.0/383.0(GC), m/z 325.0/163.1(BB), m/z 301.0/150.9(QCT), m/z 315.1/300.0(ISR), m/z 284.9/93.0(KAE)。结果:在7 min内舒血宁注射液中萜类内酯和黄酮类成分完全分离;峰面积与浓度呈良好的线性关系;加样回收率为97.7%~101.5%, 精密度RSD为0.57%~1.20%。结论:建立测定舒血宁注射液中7个成分含量的方法, 具有良好的重复性、回收率和精密度, 可用于舒血宁注射液的质量控制。

Objective:To develop an HPLC-MS method for the determination of ginkgolide A(GA),ginkgolide B(GB),ginkgolide C(GC),bilobalide(BB),quercetin(QCT),isorhamnetin(ISR)and kaempferol(KAE)in Shuxuening injection.Methods:The samples were separated on a Dikma Diamonsil C₁₈ column(150 mm×4.6 mm, 5 μm)with a mobile phrase of acetonitrile and water containing 0.05% formic acid in a gradient elution at a flow rate of 0.8 mL·min^-1,and the injection volume was 10 μL.The column temperature was set at 30℃.Multiple-reaction monitoring(MRM)scanning was employed for quantification with switching electrospray ion source polarity in negative mode.The ion spray voltage was set to -4.5 kV and the turbo spray temperature was maintained at 650℃.The precursor-to-product ion pairs of seven analytes were m/z 453.1/351.2 for GA, m/z 423.1/367.0 for GB,m/z 439.0/383.0 for GC, m/z 325.0/163.1 for BB, m/z 301.0/150.9 for QCT, m/z 315.1/300.0 for ISR andm/z 284.9/93.0 for KAE,respectively.Results:The complete separation was obtained within 7 min for the seven compounds.The regression equations showing good linear relationships between peak areas and contents of each compound were obtained.The average recoveries of the compounds ranged from 97.7% to 101.5% and the precision in terms of RSD was in the range of 0.57%-1.20%.Conclusion:The method can detect the contents of 7 components in Shuxuening injection with good repeatability,recovery and precision,and can be used for the quality control of Shuxuening injection.