高效液相色谱-串联质谱法同时测定保健食品中淫羊藿苷、金丝桃苷、补骨脂素

Simultaneous determination of icariin, hyperoside and psoralen in functional food by high performance liquid chromatography- tandem mass spectrometry

中文关键词:  保健食品  高效液相色谱-串联质谱法  淫羊藿苷  金丝桃苷  补骨脂素

英文关键词:functional food  high performance liquid chromatography-tandem mass spectrometry  icariin  hyperoside  psoralen

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定保健食品中淫羊藿苷、金丝桃苷、补骨脂素的分析方法。方法 样品经70%甲醇提取后, 采用0.1%甲酸(A)和乙腈(B)作为流动相进行梯度洗脱, 质谱离子源选用电喷雾离子(electron spray ionization, ESI+)源, 采用多离子检测模式(multiple reaction monitoring, MRM)对定量离子和定性离子进行监测, 在液相色谱-串联质谱仪上测定。结果 在15 min内完成3种目标化合物的分离分析。3种功能成分在0.25、0.5和5 mg/kg添加水平的回收率为84.3%~95.0%, 相对标准偏差为0.67%~2.11%(n=7), 方法检出限分别为0.05、25、10 μg/kg。结论 该方法快速、准确、灵敏, 适合保健食品中淫羊藿苷、金丝桃苷、补骨脂素的同时检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of icariin, hyperoside and psoralen in functional food by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Samples were extracted with 70% methanol solution, and 0.1% formic acid (A) and acetonitrile (B) as mobile phase were used for gradient elution. The electron spray ionization (ESI+) source was selected for mass spectrometry ion source, and the quantitative ion and qualitative ions were monitored by multiple reaction monitoring (MRM), and determined by HPLC-MS/MS. Results This method completed the separation and analysis of 3 target compounds in 15 minutes. The recoveries were ranged from 84.3% to 95.0% for the 3 kinds of target compound with 3 spiked levels of 0.25, 0.5 and 5 mg/kg. The relative standard deviations (RSDs) were from 0.67% to 2.11% (n=7), and the limits of detection (LOD) for the 3 kinds of target compound were 0.05, 10, 25 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting icariin, hyperoside and psoralen in functional food.