色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
7期
767-772
,共6页
邢倩倩%傅青%金郁%梁鑫淼
邢倩倩%傅青%金鬱%樑鑫淼
형천천%부청%금욱%량흠묘
反相色谱%亲水色谱%三萜皂苷%桔梗%制备
反相色譜%親水色譜%三萜皂苷%桔梗%製備
반상색보%친수색보%삼첩조감%길경%제비
reversed phase liquid chromatography ( RPLC )%hydrophilic interaction liquid chromatography( HILIC)%triterpene saponin%Platycodon grandiflorum%preparation
建立了亲水/反相二维色谱用于制备桔梗中三萜皂苷单体的方法。桔梗经水煮醇沉、反相和亲水两种模式的固相萃取后得到三萜皂苷类组分。选定 XAmide色谱柱(150 mm×20 mm,5μm),以乙腈和水为流动相,在亲水色谱模式下进行组分制备。选择时间触发模式,以1 min为单位进行馏分收集,得到6~25 min 之间的20个三萜皂苷精细组分。以第18个馏分(JG23)为例,在反相色谱模式下采用 Atlantis Prep T3色谱柱(100 mm×30 mm,5μm)制备,得到两个单体化合物。通过质谱和核磁共振对其进行定性,确定分别为deapi-platycoside E和platyco-side E。实验结果表明,该制备方法具有好的正交选择性,对于复杂样品中三萜皂苷类化合物的分离纯化有一定的借鉴意义。
建立瞭親水/反相二維色譜用于製備桔梗中三萜皂苷單體的方法。桔梗經水煮醇沉、反相和親水兩種模式的固相萃取後得到三萜皂苷類組分。選定 XAmide色譜柱(150 mm×20 mm,5μm),以乙腈和水為流動相,在親水色譜模式下進行組分製備。選擇時間觸髮模式,以1 min為單位進行餾分收集,得到6~25 min 之間的20箇三萜皂苷精細組分。以第18箇餾分(JG23)為例,在反相色譜模式下採用 Atlantis Prep T3色譜柱(100 mm×30 mm,5μm)製備,得到兩箇單體化閤物。通過質譜和覈磁共振對其進行定性,確定分彆為deapi-platycoside E和platyco-side E。實驗結果錶明,該製備方法具有好的正交選擇性,對于複雜樣品中三萜皂苷類化閤物的分離純化有一定的藉鑒意義。
건립료친수/반상이유색보용우제비길경중삼첩조감단체적방법。길경경수자순침、반상화친수량충모식적고상췌취후득도삼첩조감류조분。선정 XAmide색보주(150 mm×20 mm,5μm),이을정화수위류동상,재친수색보모식하진행조분제비。선택시간촉발모식,이1 min위단위진행류분수집,득도6~25 min 지간적20개삼첩조감정세조분。이제18개류분(JG23)위례,재반상색보모식하채용 Atlantis Prep T3색보주(100 mm×30 mm,5μm)제비,득도량개단체화합물。통과질보화핵자공진대기진행정성,학정분별위deapi-platycoside E화platyco-side E。실험결과표명,해제비방법구유호적정교선택성,대우복잡양품중삼첩조감류화합물적분리순화유일정적차감의의。
A two-dimensional(2-D)preparative liquid chromatography method was developed for the preparation of triterpene saponins from Platycodon grandiflorum using hydrophilic interaction liquid chromatography( HILIC)coupled with reversed phase liquid chromatography ( RPLC). At first,the crude extract was obtained from Platycodon grandiflorum by boiled alco-hol precipitation. Then,the concentrated crude extracts were continuously pretreated using sol-id phase extraction( SPE)under reversed-phase and hydrophilic-phase modes to remove the impurities. Subsequently,XAmide column(150 mm×20 mm,5 μm)was selected to separate the triterpene saponin constituents under HILIC mode using water and acetonitrile as mobile phases. From 6 min to 25 min,each fraction was collected per minute under time-triggered mode and 20 fractions were collected. The 18th fraction( JG23)was selected for further purifi-cation. The column of Atlantis PrepT3(100 mm×30 mm,5 μm)was chosen and two monomer-ic compounds were obtained. The two compounds with over 90% purity were identified as dea-pi-platycoside E and platycoside E with mass spectrometry( MS)and nuclear magnetic reso-nance( NMR). This 2-D HILIC-RPLC method with high orthogonality can be used in the prepa-ration of triterpene saponins from natural products.