液相色谱-质谱联用同时测定宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的含量

目的：建立宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的含量测定方法。方法：采用Agilent Eclipse XDB-C₁₈色谱柱（150 mm×2.1 mm，5.0 μm），流动相A为0.1%甲酸-10%甲醇，B为甲醇，梯度洗脱，流速为0.6 mL·min^-1；进样量10 μL，柱温30℃；采用电喷雾离子源（ESI）、正、负离子模式监测，多反应监测模式用于定量分析，喷雾电压-4.0 kV，干燥气温度为350℃，干燥气流量为11 L·min^-1，雾化器压力为0.31 MPa。结果：没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷分别在500.0~5 000、51.00~510.0、9.000~90.00、1 034~10 340 ng·mL^-1内与峰面积呈良好线性关系。宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的平均加样回收率在97%~100%之间。3批宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的含量分别为3.43~4.13、0.255~0.649、0.033 8~0.068 7、2.26~3.59 mg·g^-1。结论：经方法学验证，本方法简单、快速、灵敏，重复性好，可以用于宁泌泰胶囊的含量测定。

Objective: To develop a method for determination of gallic acid,berberine hydrochloride,palmatine hydrochloride,forsyth in Ningmitai capsules.Methods: Analysis was performed on an Agilent Eclipse XDB-C₁₈(150 mm×2.1 mm,5.0 μm)with a gradient elution.The mobile phase consisted of 0.1% formic acid-10% methanol(A)and methanol(B)and at a flow rate of 0.6 mL·min^-1. The injection volume was 10 μL,and the column temperature was controlled at 30℃.The multiple-reaction monitoring scanning was employed for the quantification with switching electrospray ion source polarity in positive and negative mode.The capillary voltage was -4.0 kV,gas temperature was 350℃,gas flow was 11 L·min^-1 and nebulizer pressure was set at 0.31 MPa.Results: The linear ranges for gallic acid,berberine hydrochloride,palmatine hydrochloride,and forsyth were 500.0-5 000,51.00-510.0,9.000-90.00,and 1 034-10 340 ng·mL^-1,respectively.The recoveries were between 97%~100%.The contents of gallic acid,berberine hydrochloride,palmatine hydrochloride,and forsyth were 3.43-4.13,0.255-0.649,0.033 8-0.068 7,and 2.26-3.59 mg·g^-1,respectively.Conclusion: The method validated was convenient,rapid,sensitive and accurate.