[关键词]
[摘要]
建立一种微波辅助离子液体均相液液微萃取高效液相色谱-串联质谱法,测定了中药材厚朴中的厚朴酚与和厚朴酚。本研究以离子液体为萃取溶剂,样品经微波提取后,向所获得的样品提取液中加入离子对试剂六氟磷酸铵(NH4PF6),采用均相液液微萃取法分离富集目标分析物,并通过高效液相色谱-串联质谱进行定性定量检测。本研究对影响萃取效率的各个条件进行单因素和响应面优化。实验结果表明,目标分析物在检测浓度范围内具有较好的线性关系(R>0.9999),检出限和定量限分别为17.2~3.9 ng/g和57.4~79.6 ng/g,样品加标回收率在89.25%~95.00%之间。与传统超声提取法和回流提取法相比,本法在溶剂用量、萃取时间上具有一定的优势,可用于中草药及相关医药产品中厚朴酚与和厚朴酚的提取分析。
[Key word]
[Abstract]
Microwave-assisted ionic liquid homogeneous liquid-liquid microextraction combined with high performance liquid chromatography tandem mass spectrometry was established to extract magnolol and honokiol from Magnolia officinalis Rehd. et Wils. In this study, ionic liquid was used as the extraction solvent. After microwave-assisted extraction, the ion-pairing reagent, ammonium hexafluorophosphate (NH4PF6), was added to the obtained sample extract, and the target analytes were separated and enriched by homogeneous liquid-liquid microextraction, and analyzed qualitatively and quantitatively by high performance liquid chromatography-tandem mass spectrometry. In this study, the conditions affecting the extraction efficiency were optimized by single factor and response surface experiments. The experimental results showed a good linear relationship (R>0.9999) for the target analytes within the detection concentration range, with the limit of detection (LOD) and limit of quantitation (LOQ) being 17.2~23.9 ng/mL and 57.4~79.6 ng/mL, respectively, and the spiked recovery between 89.25% and 95.00%. Compared with the traditional ultrasonic extraction and reflux extraction methods, the present method has advantages in the amount of solvent used and extraction time, and can be used for the extraction of magnolol and honokiol in Chinese herbal medicine and related pharmaceutical products.
[中图分类号]
[基金项目]
国家自然科学基金青年科学基金项目(21401011);吉林省教育厅“十三五”科学技术项目(JJKH20181014K)