LC-MS测定附子理中丸中3种双酯型生物碱含量

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Polaris C₁₈-A(50 mm×2.0 mm,5 μm)色谱柱,流动相为甲醇-水(90∶ 10),流速0.2 mL·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0.232~1.392 μg·mL^-1(r=0.9997)、0.102~0.612 μg·mL^-1(r=0.9994)和0.241~1.446 μg·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.