UPLC-ELSD法同时测定伊贝母中贝母辛和西贝母碱的含量

Simultaneous determination of peimisine and sipeimine in Fritillaria walujewii Regel and Fritillaria pallidiflora Schrenk by UPLC-ELSD

建立同时快速测定伊贝母两种基原植物中贝母辛和西贝母碱含量的方法。采用超高效液相色谱-蒸发光散射(UPLC-ELSD)检测法:色谱柱为Waters Acquity UPLCTM BEH C18(100 mm×2.1 mm,1.7μm);流动相为乙腈(A)-0.02%三乙胺水溶液(B)系统;梯度洗脱(0～3 min,30%～60%A;3～4 min,60%～80%A;4～10 min,80%～100%A)。流速0.25 mL.min-1;柱温25℃;漂移管温度40℃,喷雾器参数40%,进样量1μL。贝母辛和西贝母碱分别在28.75～1150.0μg.mL-1(r=0.999 2)、51.5～1 030.0μg.mL-1(r=0.999 1)内浓度对数与峰面积对数呈良好线性关系,方法回收率分别为94.5%(RSD=1.12%)和98.1%(RSD=2.36%)。结果表明,本方法快速、简便、准确、重现性好,能快速分析伊贝母药材中两种生物碱含量,为伊贝母药材的质量控制提供了依据,此外,从UPLC-ELSD色谱图能快速鉴别新疆贝母和伊犁贝母药材。

The paper reports the establishment of a method for simultaneous determination of peimisine and sipeimine contents in Fritillaria walujewii Regel and Fritillaria pallidiflora Schrenk.The analyses were performed on an ultra-performance liquid chromatography with evaporative light scattering detection（UPLC-ELSD）,equipped with a binary solvent manager,a sampler manager and a column compartment,and connected to Waters Empower 2 software.An Acquity UPLCTM BEH C18 column（100 mm × 2.1 mm,1.7 μm） was used for all analysis.The investigated compounds were separated with gradient mobile phase consisting of acetonitrile-0.02% triethylamine-water.The temperature of sample manager was set at 25 ℃.Drift tube temperature was 40 ℃,and spray parameter was 40% with injection volume of 1 μL.The investigated compounds including peimisine and sipeimine had good linearity（r ≥ 0.9991） over the tested ranges.The average recovery was 94.5% and 98.1% with RSD ≤ 2.36%.The UPLC-ELSD method is simple,sensitive and accurate with good repeatability,which is available for quality control of F.walujewii Regel and F.pallidiflora Schrenk.