液相色谱-串联质谱法测定植物来源保健食品中去甲乌药碱

Determination of higenamine in plant-derived health food by liquid chromatography-tandem mass spectrometry

中文关键词:  去甲乌药碱  液相色谱-串联质谱法  植物来源保健食品

英文关键词:higenamine  liquid chromatography-tandem mass spectrometry  plant-derived health food

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测植物来源保健食品中去甲乌药碱的分析方法。方法 样品经甲醇溶液超声提取, 采用0.1%甲酸(A)和甲醇(B)作为流动相进行梯度洗脱, 采用LC-MS/MS进行测量, 采用正离子源模式(positive electrospray ionization, ESI+)和多离子监测模式(multiple reaction monitoring, MRM)。结果 去甲乌药碱在上述色谱条件下能完全分离。去甲乌药碱线性范围为5.34~106.8 ng/mL, 相关系数r2=0.9999, 方法检出限为2 μg/kg, 定量限为 6 μg/kg; 平均回收率98.7%~101.3%, 相对标准偏差(relative standard deviation, RSD)＜2.0%。结论 该方法操作简便, 精密度和回收率高, 重复性好, 可以用于测定植物来源保健食品中去甲乌药碱。

英文摘要:

      Objective To establish a method for determination of higenamine in plant-derived health food samples by liquid chromatography-tandem mass spectrometric (LC–MS/MS). Methods The samples were ultrasonically extracted with methanol solution, using a gradient elution program of 0.1% formic acid aqueous solution (A) and methanol (B). LC-MS/MS was used for the measurement with positive ion source mode (ESI+) and multiple reaction monitoring (MRM) mode. Results Higenamine was completely separated in the chromatographic conditions. The linear range was 5.34–106.8 ng/mL, with the correlation coefficient r2=0.9999. The limit of detection was 2 μg/kg, and the limit of quantification was 6 μg/kg. The average recoveries were 98.7%–101.3%, with relative standard deviation (RSD)＜2.0%. Conclusion This method is simple, accurate and reproducible, which can be used for the determination of higenamine in health food from plants.