报告人:陈宗保 单位 : 上饶师范学院

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上饶师范学院,化学化工学院. 报告人:陈宗保 单位 : 上饶师范学院. 有机聚合物毛细管电色谱整体柱的制备及其药物分析中的应用研究. 主要内容. 1. 研究背景. 2. 目前研究工作进展. 研究背景. 20 世纪五十年代, Mould 和 Synge 首次在簿层色谱中加入电场分离胶棉中糖类化合物. 1981 年 ,Jorgenson 和 Lukacs 的毛细管填充了 10 μm 粒径 ODS ,在电场作用下成功分离了 9- 甲基蒽和芘,获得了 31000 理论塔板数的柱效,具有重要意义。. - PowerPoint PPT Presentation

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  • 1. 2.

  • 1981,JorgensonLukacs10 m ODS9-31000 2090CEC 21 20MouldSynge.

  • CECCEC,

  • 1.2

  • 1.4

  • 1 (LMA-co-EDMA)

    2 (SMA-TRIMA)

    3

  • 1.LMA-co-EDMA1.1 1-21-1

  • 1.2 2-1 2-2

  • (a) (b) (c) (d) (e) (f)2-3 SEM (a) 2h, (b) 5h, (c)10h, (d) 12h, (e) 15h, (f) 20h

  • 1.3 1.3.1 2-4 SEM(a) 800, (b) 3000, (c) 5000

  • 1.3.2 1.3.2.1 1-3 / pH 7.0 10 mmol/L (v/v) pH: pH2.53.0EOF0.88 mm/s1.15 mm/spH>3.0EOFpH

  • 1.3.2.2 .2-3 2-6

  • 2-7

  • 1.4 -CEC2, pH2 2-9 pH2-8 1.4.1

  • 1.4.2 2-11 2-12 2-10 21. 2. 3. 4536320

  • 1.4.3 2-4

  • 1.4.4 2-5 22-13 a(0 h);b(2 h);

  • 2.2 (SMA-co-TMPTMA)SMA/TMPTMA=3/2v/v;(/1,4-/=66.7/23.3/10)=6/4;(AIBN)(g)/AMPS(g)/(mL)=4.0/1.2/100(w/w/v);2-1 (SMA-co-TMPTMA)2-2

  • 2.3 2-3 1 ; 2 ; 3 N6 -; 4 ; 5

  • 2.3.1 2-4 2-5 Peak: 1 adenine, 2 guanine, 3 N6- methyladenosine, 4 adenosine, 5 cytidine

  • 2-6 pH2-7 Peak: 1 adenine, 2 guanine, 3 N6- methyladenosine, 4 adenosine, 5 cytidine

  • 2-9 CEC conditions: mobile phase, pH 5.5, 6.0 mmol/L broax buffer; applied voltage, 15 kV; sample injection, 10 kV/5 s detection wavelength, 210 nm2-8 Peak: 1 adenine, 2 guanine, 3 N6- methyladenosine, 4 adenosine, 5 cytidine

  • 3-3 2.3.2

    CompoundRegression equationR2Line rangeg/mLDetection limit(g/mL)

    Adenine y=1.3432x+4.76590.99490.5~50.00.50Guanine y=0.9735x+2.22480.99341.0~100.00.20N6-Methyladenosine y=1.2132x+3.13230.99871.0~100.00.50Adenosine y=1.3486x+4.13720.99211.0~100.00.25Cytidine y=0.8764x+4.35320.99171.0~100.00.50

  • 2.3.3 3-4 (n=3)

    CompoundAdded(g/mL)Found(g/mL)Recovery(%)RSDn=3(%)Adenine10.09.5595.503.6330.028.193.672.12Guanine10.010.53105.34.2150.049.8599.703.38N6-Methyladenosine10.08.9789.702.2850.051.35102.73.75Adenosine10.011.33113.34.3850.048.7497.484.76Cytidine10.08.8988.903.7350.051.76103.54.25

  • 4.1 4-1 4-1 3.1

  • 3.2 4-2 (a)1000; (b) 3000;(c) 5000 (b) (c) (a)

  • 4-340%45%47.5%50%55%.3.3 3.3.1 1 aniline, 2 naphthylamine3 diphenylamine4 DMA5 thiourea

  • 3.3.2 pH4-4 pH3.05.06.58.09.0.1 aniline, 2 naphthylamine3 diphenylamine4 DMA5 thiourea

  • 3.3.3 4-5 5.0101520.1 aniline, 2 naphthylamine3 diphenylamine4 DMA5 thiourea

  • 3.5 3.5.1ACN4-6 4-770%65%60%55%.1 piperine; 2nuciferine; 3 kokuline; 4berberine; 5 Tetrandrine

  • 3.5.2 pH4-8pH5.56.88.5.3.5.3 4-918151210.

  • 3.5.4 4-2

  • 3.5.5 3.5.6 4-104-11

  • pH