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
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
复制标题
微基质固相分散体耦合MEEKC以TS-1分子筛为吸附剂定量分析五味子中的木脂素
DOI：
10.1016/j.jchromb.2017.08.024
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发表时间：
2017-09-15
影响因子：
3
通讯作者：
Yan, Jizhong
中科院分区：
文献类型：
--
作者：
Chu, Chu;Wei, Mengmeng;Yan, Jizhong
建立了微基质固相分散(MSPD)与微乳电动色谱联用(MEEKC)测定五味子中木脂素的简便、有效的方法。首次将TS-1分子筛作为固体载体应用于微量MSPD的萃取。对影响萃取效率的分散剂种类、样品与分散剂的质量比、研磨时间、洗脱溶剂和体积等参数进行了优化。最佳提取工艺条件为：将25 mg五味子药材与50 mg TS-1药材混合，用研钵和砧头分散。研磨时间采用150 S。然后将混合物转移到固相萃取柱中，目标分析物用500毫升的甲醇洗脱。此外，还研究了影响MEEKC分离的几个参数，包括油的种类、十二烷基硫酸钠的浓度、助表面活性剂的种类和浓度、有机改性剂的浓度。线性关系良好(R>；0.9998)，定量限小于2.77mg/mL。最后，将微型MSPD-MEEKC方法成功地应用于五味子药材中木脂素的分析。
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 1, 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 (R > 0.9998) was obtained, and the calculated limits of quantitation were less than 2.77 mu g/mL. Finally, the micro MSPD-MEEKC method was successfully applied to the analysis of lignans in complex Schisandrae fructus samples.