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Microwave-Assisted Extraction Followed by Solid-Phase Extraction for the Chromatographic Analysis of Alkaloids in Stephania cepharantha

机译:微波辅助萃取-固相萃取对头孢石楠生物碱的色谱分析

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摘要

A procedure involving microwave-assisted extraction (MAE) followed by solid-phase extraction (SPE) was established for the extraction and purification of three bisbenzylisoquinoline alkaloids from Stephania cepharantha, and a reversed-phase high-performance liquid chromatography (HPLC) method was developed for the quantification of the target alkaloids. Chromatographic separation was achieved on a Phenomenex Luna Phenyl-Hexyl column. Prior to the HPLC analysis, the alkaloids were rapidly extracted by an optimized MAE process using 0.01 mol/L hydrochloric acid as the solvent. The MAE extract was subsequently purified by SPE using a cation-exchange polymeric cartridge. The MAE–SPE procedure extracted the three alkaloids with satisfactory recoveries ranging from 100.44 to 102.12%. In comparison with the MAE, Soxhlet and ultrasonic-assisted extractions, the proposed MAE–SPE method showed satisfactory cleanup efficiency. Thus, the validated MAE–SPE–HPLC method is specific, accurate and applicable to the determination of alkaloids in S. cepharantha.
机译:建立了微波辅助提取(MAE)然后固相提取(SPE)的方法,用于从头孢Stephania cepharantha中提取和纯化三种双苄基异喹啉生物碱,并开发了反相高效液相色谱(HPLC)方法用于目标生物碱的定量。在Phenomenex Luna苯基己基色谱柱上完成色谱分离。在进行HPLC分析之前,使用0.01 mol / L盐酸作为溶剂,通过优化的MAE工艺快速提取生物碱。随后使用阳离子交换聚合物柱通过SPE纯化MAE提取物。 MAE-SPE方法提取了三种生物碱,回收率从100.44%到102.12%不等。与MAE,索氏提取和超声辅助提取相比,所提出的MAE–SPE方法显示出令人满意的净化效率。因此,经过验证的MAE-SPE-HPLC方法具有特异性,准确性,可用于测定头孢链霉菌中的生物碱。

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