固相萃取-超高效液相色谱-串联质谱法测定菊花中15种吡咯里西啶生物碱毒素

Determination of 15 kinds of pyrrolizidine alkaloids in Chrysanthemum by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  吡咯里西啶生物碱毒素  UPLC-MS/MS  Oasis PRiME MCX固相萃取小柱  菊花

英文关键词:pyrrolizidine alkaloids  ultra performance liquid chromatography-tandem mass spectrometry  Oasis PRiME MCX solid phase extraction  Chrysanthemum

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定菊花中15种吡咯里西啶生物碱毒素含量的分析方法。方法 样品中吡咯里西啶生物碱毒素采用0.1 mol/L硫酸水溶液提取, 通过Oasis PRiME MCX固相萃取小柱净化, 采用UPLC-MS/MS进行分析。采用Acquity UPLC BEH C18色谱柱分离, 以0.1%甲酸水-甲醇溶液为流动相进行梯度洗脱, 电喷雾离子源正离子电离, 多反应离子监测模式监测, 外标法定量。结果 15种吡咯里西啶生物碱毒素在一定浓度范围内线性关系良好, 相关系数(r2)均大于0.999; 定量限为0.50~10.00 μg/kg, 检出限为0.15~3.00 μg/kg; 阴性样品的加标回收率为82.8%~92.4%, 相对标准偏差为2.1%~4.9% (n=5)。结论 该方法准确度和精密度高, 耗时短, 能同时测定多种菊花样品中的多种吡咯里西啶生物碱毒素含量。

英文摘要:

      Objective To establish a method for determination of 15 kinds of pyrrolizidine alkaloids in Chrysanthemum by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Pyridolizidine alkaloid toxins in the sample were extracted with 0.1 mol/L sulfuric acid aqueous solution and purified by Oasis PRiME MCX solid phase extraction column, detected by UPLC-MS/MS, separated by the Acquity UPLC BEH C18 column, and using the 0.1% formic acid-methanol solution as the mobile phase for gradient elution, ionized by electrospray ion source positive ion, monitored by multi-reactive ion monitoring mode, quantified by external standard method. Results Good linear relationships were seen for the 15 kinds of pyrrolizidine alkaloids in certain concentration ranges, and the correlation coefficients were more than 0.999. The limits of detection and limits of quantitation for the 15 kinds of pyrrolizidine alkaloids were in the ranges 0.15?3.00 and 0.50?10.00 μg/kg, respectively. The recoveries of negative samples ranged from 82.8% to 92.4%, and the relative standard deviations were from 2.1% to 4.9% (n=5). Conclusion The method has high accuracy, high precision and short time consuming, and can simultaneously determine the content of pyrrolizidine alkaloids in a variety of Chrysanthemum samples.