世界科学技术-中医药现代化
世界科學技術-中醫藥現代化
세계과학기술-중의약현대화
World Science and Technology-Modernization of Traditional Chinese Medicine
2015年
9期
1818-1822
,共5页
倪付勇%宋亚玲%刘露%赵祎武%洪奎%黄文哲%王振中%萧伟
倪付勇%宋亞玲%劉露%趙祎武%洪奎%黃文哲%王振中%蕭偉
예부용%송아령%류로%조의무%홍규%황문철%왕진중%소위
新绿原酸%金银花%对照品%中低压制备色谱
新綠原痠%金銀花%對照品%中低壓製備色譜
신록원산%금은화%대조품%중저압제비색보
Neochlorogenic acid%Lonicera japonica%reference substances%medium-low-pressure preparative chromatography
目的:建立从金银花中分离制备新绿原酸对照品的方法。方法:利用HPD200A大孔树脂对金银花水提液中的新绿原酸富集,经中低压制备色谱分离制备金银花中新绿原酸单体,运用HPLC对新绿原酸进行含量测定。采用现代波谱技术ESI-MS、1H-NMR、13C-NMR进行结构鉴定。结果:新绿原酸的最佳纯化工艺为加5 BV水洗脱,收集水洗液,浓缩、干燥,得新绿原酸粗品;以乙腈-0.5%甲酸溶液(10:90)为流动相,流速20 mL?min-1,检测波长326 nm,进行分离纯化,分离制备的新绿原酸的纯度达98.86%,收率为89.1%。结论:该方法可有效制备高纯度的新绿原酸对照品,以用于中药新药中定性鉴别和含量测定。
目的:建立從金銀花中分離製備新綠原痠對照品的方法。方法:利用HPD200A大孔樹脂對金銀花水提液中的新綠原痠富集,經中低壓製備色譜分離製備金銀花中新綠原痠單體,運用HPLC對新綠原痠進行含量測定。採用現代波譜技術ESI-MS、1H-NMR、13C-NMR進行結構鑒定。結果:新綠原痠的最佳純化工藝為加5 BV水洗脫,收集水洗液,濃縮、榦燥,得新綠原痠粗品;以乙腈-0.5%甲痠溶液(10:90)為流動相,流速20 mL?min-1,檢測波長326 nm,進行分離純化,分離製備的新綠原痠的純度達98.86%,收率為89.1%。結論:該方法可有效製備高純度的新綠原痠對照品,以用于中藥新藥中定性鑒彆和含量測定。
목적:건립종금은화중분리제비신록원산대조품적방법。방법:이용HPD200A대공수지대금은화수제액중적신록원산부집,경중저압제비색보분리제비금은화중신록원산단체,운용HPLC대신록원산진행함량측정。채용현대파보기술ESI-MS、1H-NMR、13C-NMR진행결구감정。결과:신록원산적최가순화공예위가5 BV수세탈,수집수세액,농축、간조,득신록원산조품;이을정-0.5%갑산용액(10:90)위류동상,류속20 mL?min-1,검측파장326 nm,진행분리순화,분리제비적신록원산적순도체98.86%,수솔위89.1%。결론:해방법가유효제비고순도적신록원산대조품,이용우중약신약중정성감별화함량측정。
This study was aimed to establish a separation method for neochlorogenic acid reference substances from Lonicera japonica. Refined neochlorogenic acid inL. japonica water extract was separated and concentrated by HPD200A macroporous resin, which was isolated and purified by medium-low-pressure preparative chromatography and determined by HPLC. The structure was identified by various spectroscopic data including ESI-MS,1H-NMR and13C-NMR. The results showed that the optimal purification technology conditions were as follows: washed with 5BV of water, collected elution, concentration, drying; neochlorogenic acid crude products were eluted with acetonitrile-0.5% formic acid solution (10:90) with the flow rate of 20 mL·min-1; and the detection wavelength was 326 nm. The contents of the prepared neochlorogenic acid reached to 98.86% and the yield was 89.1%. It was concluded that the method was effective for the preparation of neochlorogenic acid with high purity. It can be used to prepare the reference substances for quantitative analysis and content determination of Chinese materia medica.