[关键词]
[摘要]
目的 建立UPLC-MS/MS方法同时测定木蝴蝶中木蝴蝶苷A、木蝴蝶苷B、黄芩苷、黄芩素、白杨素、高车前素、野黄芩素、金丝桃苷、芹菜素、槲皮素10种主要成分。方法 采用负离子多反应监测(MRM)模式,ESI离子源,Kinetex C18色谱柱(100 mm×3.0 mm,2.6 μm)进行分离,流动相为乙腈-甲醇-0.5%甲酸水,梯度洗脱,分析时间为7 min。结果 所测10种主要成分在测定浓度范围内线性关系良好,相关系数均大于0.996 6;精密度、重复性和稳定性良好;平均加样回收率为94.0%~104.5%,RSD≤3.21%。结论 首次建立可同时测定木蝴蝶中10种主要成分的UPLC-MS/MS方法,该法操作简便,灵敏度高,专属性好,分析速度快,可用于中药材木蝴蝶的质量控制。
[Key word]
[Abstract]
Objective To develop and validate an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of ten component (baicalin-7-glucoside, oroxin BCAS, baicalin, baicalein, chrysin, hispidulin, scutellarein, hyperoside, apigenin and quercetin) in Oroxylum indicum. Methods The ten components were separated within 7.0 min on a Kinetex C18 column (100 mm×3.0 mm, 2 μm) using a mobile phase consisted of methanol, acetonitrile and 0. 1% formic acid water solution with gradient elution. Results All of the analytes showed good linearity (r ≥ 0. 996 6) in the tested ranges. The precision, repeatability and stability of the method were good for the ten components. The average recoveries were in the range of 94.0%-104.5% with relative standard deviations (RSD) ≤ 3.21%. Conclusion A new rapid and reliable UPLC-MS/MS method was developed and validated to evaluate the quality of O. indicum for the first time.
[中图分类号]
R286.2
[基金项目]
河北省卫计委课题(20170287);河北省高等学校科学技术研究重点项目(ZD2019054);河北省自然科学基金面上项目(H2019206219)