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Micro-matrix solid-phase dispersion coupled with MEEKC for quantitative analysis of lignans in Schisandrae Chinensis Fructus using molecular sieve TS-1 as a sorbent
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-08-24 , DOI: 10.1016/j.jchromb.2017.08.024
Chu Chu , Mengmeng Wei , Shan Wang , Liqiong Zheng , Zheng He , Jun Cao , Jizhong Yan

A simple and effective method was developed for determining lignans in Schisandrae Chinensis Fructus by using a micro-matrix solid phase dispersion (MSPD) technique coupled with microemulsion electrokinetic chromatography (MEEKC). Molecular sieve, TS-1, was applied as a solid supporting material in micro MSPD extraction for the first time. Parameters that affect extraction efficiency, such as type of dispersant, mass ratio of the sample to the dispersant, grinding time, elution solvent and volume were optimized. The optimal extraction conditions involve dispersing 25 mg of powdered Schisandrae samples with 50 mg of TS-1 by a mortar and pestle. A grinding time of 150 s was adopted. The blend was then transferred to a solid-phase extraction cartridge and the target analytes were eluted with 500 μL of methanol. Moreover, several parameters affecting MEEKC separation were studied, including the type of oil, SDS concentration, type and concentration of cosurfactant, and concentration of organic modifier. A satisfactory linearity (> 0.9998) was obtained, and the calculated limits of quantitation were less than 2.77 μg/mL. Finally, the micro MSPD-MEEKC method was successfully applied to the analysis of lignans in complex Schisandrae fructus samples.



中文翻译:

微基质固相分散体与MEEKC结合使用分子筛TS-1作为吸附剂对北五味子中木脂素的定量分析

开发了一种简单有效的方法,通过使用微基质固相分散体(MSPD)技术与微乳液电动色谱(MEEKC)结合来测定五味子中的木脂素。TS-1分子筛首次用作微型MSPD萃取中的固体支持材料。优化了影响萃取效率的参数,例如分散剂的类型,样品与分散剂的质量比,研磨时间,洗脱溶剂和体积。最佳提取条件包括分散25毫克五味子用研钵和研棒将样品中含有50 mg TS-1。采用150 s的研磨时间。然后将共混物转移到固相萃取柱中,并用500μL甲醇洗脱目标分析物。此外,研究了影响MEEKC分离的几个参数,包括油的类型,SDS浓度,助表面活性剂的类型和浓度以及有机改性剂的浓度。获得了令人满意的线性度( > 0.9998),计算的定量限小于2.77μg/ mL。最终,微型MSPD-MEEKC方法成功地用于五味子五味子样品中木脂素的分析。

更新日期:2017-08-24
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