固相萃取-超高效液相色谱法测定人参中5种原人参二醇型人参皂苷的含量  

Determination of five protopanaxadiol ginsenosides in ginseng by solid-phase extraction-ultra performance liquid chromatography

作　　者：宋春颖 张华蓉 郭志谋[1,3] 闫竞宇 金高娃[1,3] 梁鑫淼 SONG Chunying;ZHANG Huarong;GUO Zhimou;YAN Jingyu;JIN Gaowa;LIANG Xinmiao(Key Lab of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;University of Chinese Academy of Sciences, Beijing 100049, China;DICP-CMC Innovation Institute of Medicine, Taizhou 225300, China)

机构地区：[1]中国科学院大连化学物理研究所,中国科学院分离分析化学重点实验室,辽宁大连166023 [2]中国科学院大学,北京100049 [3]中科院大化所中国医药城生物医药创新研究院,江苏泰州225300

出　　处：《色谱》2020年第5期547-553,共7页Chinese Journal of Chromatography

基　　金：国家自然科学基金重点基金(U1508221).

摘　　要：建立了固相萃取-超高效液相色谱测定人参中5种原人参二醇型人参皂苷的方法。人参药材经粉碎后通过水饱和正丁醇溶液进行超声提取,经过亲水作用固相萃取柱净化后,在ACQUITY UPLC BEH Shield RP18色谱柱(100 mm×2.1 mm,1.7μm)上分离,利用乙腈/水作为流动相进行梯度洗脱,采用光电二极管阵列检测器检测。结果表明,5种原人参二醇型人参皂苷在5~500μg/mL范围内具有很好的线性关系,相关系数均大于0.999。方法精密度的RSD值在0.95%~2.62%(n=6)之间,22 h内样品稳定性的RSD值在0.90%~2.15%(n=8)之间,日内和日间重复性的RSD值分别为5.35%~6.47%(n=6)和5.56%~6.34%(n=8)。方法的加标回收率在87.16%~101.92%之间,相对标准偏差在1.54%~4.01%(n=6)之间。所建立的方法采用亲水作用色谱模式的固相萃取材料,药材的提取液可直接作为固相萃取的上样溶液进行人参皂苷的富集和净化,并且超高效液相色谱大大缩短了分析时间。该方法简单快速、通量高、重现性好,适用于人参中5种原人参二醇型人参皂苷的定量分析。A new method based on solid-phase extraction-ultraperformance liquid chromatography(SPE-UPLC)was developed for the determination of five protopanaxadiol ginsenosides in ginseng.The ginsenosides were extracted from ground ginseng samples using water-saturated n-butanol and purified on a hydrophilic solid-phase extraction column.Chromatographic separation was achieved on an ACQUITY UPLC BEH Shield RP18 column(100 mm×2.1 mm,1.7μm)by linear gradient elution using an acetonitrile/water mobile phase.Five protopanaxadiol ginsenosides were detected by a photodiode array detector,and they showed a strong positive linear correlation(r2>0.999)in the range of 5-500μg/mL.In addition,the instrument precision ranged between 0.95%and 2.62%(n=6),with the sample stability between 0.90%and 2.15%(n=8)within 22 h.Intra-and inter-day repeatabilities were 5.35%-6.47%(n=6)and 5.56%-6.34%(n=8),respectively.Sample recoveries and the corresponding relative standard deviations(RSDs)were 87.16%-101.92%and 1.54%-4.01%(n=6),respectively.Hydrophilic chromatography materials were used in SPE,and the extract was directly loaded and purified without pretreatment.Besides,with the use of UPLC,the analysis time was greatly shortened.The developed method is simple and rapid,with high throughput,thus being suitable for the quantitative analysis of the five protopanaxadiol ginsenosides in ginsengs.

关 键 词：亲水作用色谱 固相萃取 超高效液相色谱 人参皂苷 人参 

分 类 号：O658[理学—分析化学]