松贝中生物碱含量测定及清洗加工方式评价

Determination the Content of Alkaloids in Fritillaria Cirrhosa and Evaluation of Cleaning and Processing Methods

目的:同时测定松贝中西贝母碱苷和西贝母碱的含量,考察不同清洗加工方式对松贝中西贝母碱苷和西贝母碱含量的影响。方法:采用UPLC-MS/MS法,流动相为乙腈-0.1%甲酸溶液(含10 mmol/L甲酸铵)梯度洗脱,流速0.4 mL/min,柱温35℃,质谱采用ESI+离子源,动态多反应监测模式检测。结果:松贝中2种生物碱成分在一定浓度范围内线性关系良好,所用方法精密度、重复性、稳定性良好,平均回收率为90.48%和93.60%,RSD<3%。不同产地松贝中西贝母碱苷和西贝母碱含量差异较大;不同清洗加工方式处理后松贝中西贝母碱和西贝母碱苷的含量具有一定差异。结论:所用方法能全面、准确地测定松贝中2种生物碱成分的含量。该研究可为松贝的质量控制、临床应用和综合评价提供参考依据。

Objective:Simultaneous determination of sipeimine-3β-D-glucoside and Sipeimine in Fritillaria cirrhosa,and to investigate the effects of different cleaning and processing methods.Methods:UPLC-MS/MS was used with gradient elution of acetonitrile-0.1%formic acid solution(containing 10mmol/L ammonium formate)as mobile phase at a flow rate of 0.4mL/min and column temperature was 35℃.The mass spectrometry parameters were electrospray ionization(ESI+)and dynamicmultiple reaction monitoring mode(DMRM).Results:The results showed that good linearity was achieved in their ranges and fine determination coefficient.The accuracy,repeatability and stability of the method were good.The average recoveries were 90.48%and 93.60%,RSD was less than 3%.The contents of sipeimine-3β-D-glucoside and Sipeimine in Fritillaria cirrhosa from different regions were different.After different cleaning and processing methods,the contents of sipeimine-3β-D-glucoside and Sipeimine in Fritillaria cirrhosa had certain differences.Conclusion:The method can be used to determine the content of alkaloids in 2 in Fritillaria cirrhosa comprehensively and accurately.It provides a scientific reference for quality control,clinical application and comprehensive assessment for Fritillaria cirrhosa.