液相色谱-串联质谱法测定曼陀罗中东莨菪碱、消旋山莨菪碱和阿托品含量

Determination of scopolamine, racanisodamine and atropine in Datura stramonium Linn. by liquid chromatography-tandem mass spectrometry

中文关键词:  LC-MS/MS  曼陀罗  东莨菪碱  消旋山莨菪碱  阿托品

英文关键词:liquid chromatography-tandem mass spectrometry  Datura stramonium Linn.  scopolamine  racanisodamine  atropine

中文摘要:

      目的 建立快速提取曼陀罗籽、曼陀罗花、曼陀罗壳、曼陀罗叶和曼陀罗茎的前处理法, 采用液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)同时检测东莨菪碱、消旋山莨菪碱和阿托品。方法 以甲醇提取曼陀罗籽, 以乙醇提取花, 以1%甲酸水提取壳、叶和茎, 选用ACQUITY UPLC BEH C18 (100 mm×2.1 mm,1.7 μm)为色谱柱, 以0.1%甲酸水溶液-甲醇为流动相梯度洗脱, 电喷雾离子源正离子扫描, 多反应监测(multiple reaction monitoring, MRM)模式采集, 外标法定量。结果 在质量浓度0.1~10.0 ng/mL范围内, 东莨菪碱、消旋山莨菪碱和阿托品呈现良好的线性关系(r≥0.999); 检出限为30~76 μg/kg, 定量限为80~253 μg/kg; 3种生物碱在低、中、高3个加标浓度水平的平均回收率为81.9%~117.0%, 相对标准偏差(relative standard deviation, RSDs)为0.7%~7.2%。结论 该方法操作简单、快速、准确, 为测定曼陀罗多种组织中东莨菪碱、消旋山莨菪碱和阿托品提供了可靠的技术支持。

英文摘要:

      Objective To establish a method for the rapid extraction of Datura stramonium Linn. seeds, Datura stramonium Linn. flowers, Datura stramonium Linn. shells, Datura stramonium Linn. leaves and Datura stramonium Linn. stems and simultaneous determination of scopolamine, racanisodamine and atropine by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The Datura stramonium Linn. seeds were extracted with methanol , flowers were extracted with ethanol and others were extracted with 1% formic acid solution. An ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm) column was used for the qualitative and quantitative analysis of scopolamine, racanisodamine and atropine by external standard method in multiple reaction monitoring (MRM) mode using 0.1% formic acid aqueous solution-methanol as the mobile phase in a gradient elution and electrospray ionization with a positive ion source. Results Scopolamine, racanisodamine and atropine showed good linearity (r≥0.999) in the range of mass concentrations from 0.1 to 10.0 ng/mL. Limits of detection were 30–76 μg/kg, limits of quantitation were 80–253 μg/kg. The average recoveries of the 3 alkaloids at the low, medium and high spiked concentration levels ranged from were 81.9%–117.0%, and the relative standard deviations (RSDs) were 0.7%–7.2%. Conclusion The method is simple, rapid, accurate, can provide reliable technical support for the determination of scopolamine, racanisodamine and atropine in Datura stramonium Linn..