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

Simultaneous determination of terpene lactones and favonoid aglycones in Shuxuening injection by HPLC-MS

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,5μm),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10μL;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/z301.0/150.9(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 Shuxu- ening 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 O. 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 -reac- tion 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, rn/z 301.0/150. 9 for QCT,m/z 315.1/300. 0 for ISR and m/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 quali- ty control of Shuxuening injection.