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目的建立测定附桂骨痛胶囊中新乌头碱、乌头碱和次乌头碱的HPLC-MS分析方法。方法采用HPLC-MS,色谱柱为Polaris C18-A柱(50 mm×2.0 mm,5μm),流动相为甲醇-水(90∶10),体积流量0.2 mL/min,质谱检测采用电喷雾电离源,正离子方式检测。结果新乌头碱、乌头碱和次乌头碱分别在0.464～3.944μg/mL(r=0.999 6)、81.6～816 ng/mL(r=0.999 4)、0.482～6.748μg/mL(r=0.999 7)线性关系良好,平均回收率分别为98.8%(RSD 3.1%)、98.1%(RSD 3.3%)、98.4%(RSD 3.3%)(n=6)。结论该方法是一种快速、灵敏、准确的分析方法,可以为附桂骨痛胶囊的质量控制提供科学依据。
OBJECTIVE To establish a HPLC-MS method for the determination of mesaconitine, aconitine and hypaconitine in Fugu Gudong Capsules. Methods HPLC-MS was used. The column was Polaris C18-A (50 mm × 2.0 mm, 5 μm). The mobile phase was methanol-water (90:10) and the volume flow rate was 0.2 mL / min. , Positive ion detection. Results The concentrations of mesaconitine, aconitine and hypaconitine in the range of 0.464 ~ 3.944μg / mL (r = 0.999 6), 81.6816ng / mL (r = 0.999 4) and 0.482 ~ 6.748μg / mL = 0.999 7). The average recoveries were 98.8% (RSD 3.1%), 98.1% (RSD 3.3%) and 98.4% (RSD 3.3%) (n = 6), respectively. Conclusion This method is a rapid, sensitive and accurate method for analysis, which can provide a scientific basis for the quality control of Fugu Goku Capsule.