LC-MS测定附子理中丸中3种双酯型生物碱含量

LC-MS determination of three diester diterpenoid alkaloids in Fuzilizhong pills

目的:建立测定附子理中丸中新乌头碱、乌头碱和次乌头碱的液相色谱-质谱分析方法。方法:采用PolarisC18-A(50mm×2.0mm,5μm)色谱柱,流动相为甲醇-水(90∶10),流速0.2mL·min-1,采用电喷雾电离源正离子质谱检测。结果:新乌头碱、乌头碱和次乌头碱浓度分别在0.232～1.392μg.mL-1(r=0.9997)、0.102～0.612μg.mL-1(r=0.9994)和0.241～1.446μg.mL-1(r=0.9996)范围内线性关系良好,平均回收率(n=6)分别为98.7%(RSD=2.9%)、98.6%(RSD=3.0%)和98.1%(RSD=3.2%)。结论:该法是一种快速、灵敏、准确的分析方法,可以为附子理中丸的质量控制提供科学依据。

Objective：To establish an LC-MS method for determining of three diester diterpenoid alkaloids in Fuzilizhong pills.Method：LC-MS was adopted.The separation was performed on Polaris C18-A（50 mm×2.0 mm,5 μm）column with the mobile phase of methanol-water（90∶10）at the flow rate of 0.2 mL·min-1.The detection was done by positive-ion electrospray ionization mass spectrometry.Results：The linear ranges were 0.232-1.392 μg·mL-1（r=0.9997）for mesaconitine,0.102-0.612 μg·mL-1（r=0.9994）for aconitine and 0.241-1.446 μg·mL-1（r=0.9996）for hypaconitine,respectively.The average recoveries（n=6）were 98.7%（RSD=2.9%）for mesaconitine,98.6%（RSD=3.0%）for aconitine and 98.1%（RSD=3.2%）for hypaconitine,respectively.Conclusion：The method is rapid,sensitive and accurate for the determination of mesaconitine,aconitine and hypaconitine in Fuzilizhong pills.The study may provide a scientific basis for the quality control of Fuzilizhong pills.