Engineering Research Center of Pharmaceutical Process Chemistry, Ministry of Education, School of Pharmacy, East China University of Science and Technology, Shanghai, P. R. China.
Analytical Instruments Department, Analytical Applications Center, Shimadzu (China) Co., LTD. Shanghai Branch, Shanghai, P. R. China.
J Sep Sci. 2019 Jul;42(14):2444-2454. doi: 10.1002/jssc.201900222. Epub 2019 Jun 24.
An online supercritical fluid extraction with supercritical fluid chromatography system could provide sequential extraction and quantitative analysis of lignans in Schisandra chinensis. Supercritical fluid extraction conditions were optimized at 15 MPa, 50°C, and 4 min with supercritical CO adding 1% methanol; the elution volume and flow rate were set at 6 mL and 2 mL/min to blow extract out of the tank completely. The split-flow rate was confirmed at 2.5%, which determines injection volume and accuracy of quantitative detection. The factors having negative influences on supercritical fluid chromatography retention in the online system, including sample loading forms and backpressure settings, are discussed in the paper. At last, an extraction-quantitative method for lignans in Schisandra chinensis was developed, which could be finished within 19.5 min. The total content percentage of four lignans (Schisandrin, Schisandrin A, Schisandrin B and Schisandrol B) in four batches was respectively measured to be 1.42, 1.54, 1.62, and 1.90%.
一种在线超临界流体萃取与超临界流体色谱系统可提供五味子中木脂素的顺序提取和定量分析。超临界流体萃取条件优化为 15 MPa、50°C 和 4 分钟，超临界 CO 中添加 1%甲醇；洗脱体积和流速分别设定为 6 mL 和 2 mL/min，以将提取物完全吹出罐外。分流比确定为 2.5%，这决定了进样量和定量检测的准确性。本文讨论了在线系统中超临界流体色谱保留的负面影响因素，包括样品加载形式和背压设置。最后，建立了一种五味子中木脂素的提取-定量方法，可在 19.5 分钟内完成。四批样品中四种木脂素（五味子素、五味子甲素、五味子乙素和五味子醇 B）的总含量百分比分别为 1.42%、1.54%、1.62%和 1.90%。
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