[目的]建立UHPLC-MS/MS法同时测定25批补骨脂中17种成分的含量.[方法]采用超高效液相色谱-三重四级杆串联质谱技术检测,色谱柱为Thermofisher Scientific Hypersil GOLD(100 mmx2.1 mm 1.9 μm),流动相为水(A)-乙腈(B),梯度洗脱,进样量为3 μL,流速为0.2 mL/min,柱温40℃;离子源为电喷雾离子源(ESI);在多反应检测(MRM)模式下正、负离子同时测定.[结果]补骨脂素、异补骨脂素、补骨脂酚、4,5-去氢异补骨脂定、补骨脂查尔酮、异补骨脂色烯查尔酮、补骨脂二氢黄酮甲醚、补骨脂宁、补骨脂定、补骨脂甲素、补骨脂乙素、8-甲氧基补骨脂素、异补骨脂二氢黄酮、新补骨脂异黄酮、5-甲氧基补骨脂素、巴库查尔酮、Corylifol A 17种成分线性关系良好(r＞0.99),平均加样回收率(n=6)为95.66％～101.38％,RSD为0.77％～3.04％;精密度、重复性,稳定性试验的RSD均小于2.57％,符合分析要求.含量测定显示,不同批次补骨脂中各成分含量差别较大.[结论]本实验建立的检测方法快速、准确、重复性好,可适用于补骨脂的质量控制研究.
Simultaneous quantification of 17 components in psoraleae fructus by UHPLC-MS/MS method
[Objective]To establish a UHPLC-MS/MS method for the simultaneous determination of 17 components in 25 batches of psoraleae fructus.[Methods]The UHPLC-MS/MS method was performed on Thermofisher Scientific Hypersil GOLD(100×2.1mm 1.9μm).The mobile phase was water(A)-acetonitrile(B);Gradient elution;The injection volume was 3 μL.The flow rate was 0.2 mUmin and column temperature were 40 ℃.The ion source was ESI,the ion source temperature was 500 ℃.The positive and negative ions were measured simultaneously in multiple reaction detection(MRM)mode.[Results]psoralen,isopsoralen,bakuchiol,4,5-dehydroisopsoralidin,bavachalcone,isobavachromene,bavachinin,corylin,psoralidin,bavachin,isobavachalcone,8-methoxypsoralen,isobavachin,neobavaisoflavone,5-methoxypsoralen,bakuchalone,corylifol a 17 components with good linear relationship(r＞0.99),the average recoveries(n=6)were 95.66％～101.38％,RSD was 0.77％～3.04％.RSDS of precision,repeatability and stability tests were all less than 2.57％,which met the requirements of analysis.The content determination showed that the content of each component in different batches of psoralen was different.[Conclusion]The method established in this experiment is rapid,accurate and reproducible,and can be applied to the quality control of psoraleae fructus.
万方数据
维普
