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目的:建立LC-MS/MS同时测定复方附子口服液中10个成分(毛蕊异黄酮葡萄糖苷、苯甲酰新乌头碱、苯甲酰次乌头碱、苯甲酰乌头碱、党参炔苷、新乌头碱、次乌头碱、乌头碱、黄芪甲苷和麦冬皂苷D)含量的分析方法。方法:采用Agilent SB-C18色谱柱(2.1 mm×50 mm,1.8μm),柱温为25℃,流动相A为0.05%甲酸水溶液,流动相B为0.05%甲酸甲醇溶液,梯度洗脱(0～3.5 min,40%B;3.5～4 min,40%B→70%B;4～5 min,70%B→90%B;5～6 min,90%B;6～6.1 min,90%B→40%B;6.1～7 min,40%B),流速0.3 m L·min~(-1);电喷雾离子源(ESI),正、负离子扫描方式,多反应监测扫描模式进行定量分析。结果:所测10种成分在一定范围内具有良好的线性关系,线性相关系数r均大于0.998 1,精密度、重复性、稳定性的RSD均小于3.6%;加样回收率在95.24%～104.1%,RSD均小于4.2%。3个批次双酯型生物碱(以新乌头碱、次乌头碱、乌头碱总量计)平均含量为9.29μg·mL~(-1),满足用药安全。单酯型生物碱(以苯甲酰新乌头碱、苯甲酰次乌头碱、苯甲酰乌头碱总量计)、毛蕊异黄酮葡萄糖苷、党参炔苷、黄芪甲苷、麦冬皂苷的平均含量分别为604.3、72.3、47.8、308、7.69μg·mL~(-1)。结论:所建立的分析方法经方法学验证,可为复方附子口服液的质量控制提供依据。
OBJECTIVE: To establish a LC-MS / MS method for the simultaneous determination of 10 constituents in Fufangfuzi oral liquid (calycosin glycoside, benzoyl mesaconitine, benzoyl hypaconitine, benzoyl aconitine, , Mesaconitine, hypaconitine, aconitine, astragaloside IV and mirabilis saponins D) content analysis method. METHODS: The Agilent SB-C18 column (2.1 mm × 50 mm, 1.8 μm) was used. The column temperature was 25 ℃. The mobile phase A was 0.05% formic acid and the mobile phase B was 0.05% formic acid methanol. ~ 3.5 min 40% B 3.5 ~ 4 min 40% B 70% B 4 ~ 5 min 70% B 90% B 5 ~ 6 min 90% B 6 ~ 6.1 min 90% B → 40% B; 6.1-7 min, 40% B) at a flow rate of 0.3 m L · min -1; electrospray ionization source (ESI), positive and negative ion scan mode, . Results: The 10 components tested had a good linear relationship within a certain range, the linear correlation coefficient r was greater than 0.998 1, RSD of precision, repeatability and stability were all less than 3.6%. The recoveries of samples were between 95.24% and 104.1 %, RSD are less than 4.2%. The average content of three batches of diester alkaloids (based on mesaconitine, hypaconitine, and aconitine) was 9.29 μg · mL -1, which satisfied the medication safety. Monoester alkaloids (benzoyl mesaconitine, benzoyl hypaconitine, the total amount of benzoyl aconitine), calycosin glucoside, Codonoptin, Astragaloside, Radix Ophiopogon japonicus The average contents were 604.3,72.3,47.8,308,7.69μg · mL -1. Conclusion: The established analytical method verified by methodology can provide the basis for the quality control of Fufangfuzi oral liquid.