UPLC-MS/MS法同时测定田七痛经胶囊中香蒲新苷和异鼠李素-3-O-新橙皮苷的含量

目的：建立中成药田七痛经胶囊中蒲黄的主要有效成分香蒲新苷和异鼠李素-3-O-新橙皮苷的含量测定方法。方法：采用Infiniti Lab Poroshell 120 SB-C₁₈色谱柱（2.7 μm，4.6 mm×100 mm），以乙腈为流动相A，含0.02 mol·L^-1乙酸铵的0.2%乙酸为流动相B，梯度洗脱，流速0.3 mL·min^-1；采用电喷雾离子源进行正离子模式监测，多反应监测模式（MRM）用于定量分析，雾化气压力0.28 MPa，毛细管电压3.5 kV，干燥气温度300℃，干燥气流量6 L·min^-1。结果：香蒲新苷和异鼠李素-3-O-新橙皮苷被完全分离，质量浓度分别在295.66~5 913.12 ng·mL^-1（r=0.999 7）和304.76~6 095.28 ng·mL^-1（r=0.999 1）范围内线性关系良好。实验精密度、重复性和稳定性良好，香蒲新苷和异鼠李素-3-O-新橙皮苷的平均加样回收率分别为94.5%和103.5%。3批样品中香蒲新苷和异鼠李素-3-O-新橙皮苷的含量范围分别为0.305 6~0.360 7 mg·g^-1和0.289 9~0.354 9 mg·g^-1。结论：本方法可用于田七痛经胶囊中香蒲新苷和异鼠李素-3-O-新橙皮苷的含量测定，可为田七痛经胶囊质量标准的完善提供依据。

Objective: To develop a method for determination of the main active components(typhaneoside and isorhamnetin-3-O-neohesperidoside)in Pollen Typhae in Chinese patent medicine Tianqi Tongjing capsules.Methods: The samples were separated on an Infiniti Lab Poroshell 120 SB-C₁₈ column(2.7 μm,4.6 mm×100 mm).The mobile phase consisted of acetonitrile(A)-water containing 0.02 mol·L^-1 ammonium formate and 0.2% formic acid(B)with gradient elution,and the flow rate was 0.3 mL·min^-1.Multiple-reaction monitoring(MRM)scanning was employed for quantification with electrospray ion source polarity in positive mode.The operating conditions were as follows:nebulizer pressure was 40 psi;capillary voltage was 3.5 kV;gas temp was 300℃ and gas flow was 6 L·min^-1.Results: Typhaneoside and isorhamnetin-3-O-neohesperidoside were completely separated,and the developed method showed good linearity in the range of 295.66-5 913.12 ng·mL^-1(r=0.999 7)for typhaneoside and 304.76-6 095.28 ng·mL^-1(r=0.999 1)for isorhamnetin-3-O-neohesperidoside.The precision,repeatability,and stability of the method were good.The average recoveries of typhaneoside and isorhamnetin-3-O-neohesperidoside were 94.5% and 103.5%,respectively.The content ranges in three batches of Tianqi Tongjing capsules were 0.305 6-0.360 7 mg·g^-1 and 0.289 9-0.354 9 mg·g^-1,respectively.Conclusion: The method can be used for content determination of Tianqi Tongjing capsules,and the results may provide a basis for the quality improvement of Tianqi Tongjing capsules.