Five new 6-O-prolinated monoacetylbritannilactones have been synthesized from N-acetylprolyl chlorides with 4-N,N-dimethylaminopyridine as catalyst and characterized by elemental analysis, IR, 1H NMR, 1H-1H COSY and M...Five new 6-O-prolinated monoacetylbritannilactones have been synthesized from N-acetylprolyl chlorides with 4-N,N-dimethylaminopyridine as catalyst and characterized by elemental analysis, IR, 1H NMR, 1H-1H COSY and MS. The compound 3b displayed a good biological activity for human HL-60 cell in vitro（ED50=4.6 mg/L）.展开更多
采用熔融石英毛细管,以含有50mm o l/L十二烷基硫酸钠的50mm o l/L硼酸盐缓冲液为电极缓冲液,以10mm o l/L硼酸盐缓冲液为上样缓冲液,经过对分离条件的优化,成功地建立了胶束电动毛细管色谱结合在线sw eep ing(推扫)富集技术检测中性脂...采用熔融石英毛细管,以含有50mm o l/L十二烷基硫酸钠的50mm o l/L硼酸盐缓冲液为电极缓冲液,以10mm o l/L硼酸盐缓冲液为上样缓冲液,经过对分离条件的优化,成功地建立了胶束电动毛细管色谱结合在线sw eep ing(推扫)富集技术检测中性脂溶性物质旋覆花内酯(acety lb ritann ilac tone,ABL)的实验方法。所建方法的批内、批间测定值的相对标准偏差均小于5%,灵敏度为0.005g/L,回收率大于92%;被检测样品的含量与峰面积呈良好的线性关系,相关系数为0.997 5。用所建立的方法检测了旋覆花素中ABL的含量及其在体内的动态变化,结果表明胶束电动毛细管色谱结合在线sw eep ing样品富集技术可显著提高检测的灵敏度。该方法具有操作简单、进样量小(nL级)、检测速度快等特点,弥补了毛细管电泳在测定痕量组分方面的不足。展开更多
Objective To establish a rapid method for detecting acetylbritannilactone （ABL） by online sweeping-micellar electrokinetic chromatography （MEKC） and to elevate the sensitivity of the detection. Methods The combina...Objective To establish a rapid method for detecting acetylbritannilactone （ABL） by online sweeping-micellar electrokinetic chromatography （MEKC） and to elevate the sensitivity of the detection. Methods The combination of online sweeping technique with MEKC was used to determine the content of ABL in the extract of Inula britannica in plasma of rats. Results ABL was completely separated within 15 min in running buffer and sample buffer. The optimal conditions were as follows： on uncoated fused quartz silica capillary, with separation voltage of 23 kV, capillary temperature of 25 oC, and detection wavelength of 195 nm. The regression equations revealed good linear relationships between the peak area and concentration of ABL （r = 0.998）, with the detection limits of 0.005-0.15 mg/mL. The relative standard deviations of migration time and peak areas for intra- and inter-batch were 〈 2.45% and 〈 2.26%, respectively. The recovery rate of this method was 96.3~97.2%. Conclusion This method provides some advantages in separation speed, testing sensitivity, and operating convenience, with low sample and reagent consumption. The online sweeping-MEKC is an effective method for pharmacokinetic study and analysis on tracing biological samples.展开更多
文摘Five new 6-O-prolinated monoacetylbritannilactones have been synthesized from N-acetylprolyl chlorides with 4-N,N-dimethylaminopyridine as catalyst and characterized by elemental analysis, IR, 1H NMR, 1H-1H COSY and MS. The compound 3b displayed a good biological activity for human HL-60 cell in vitro（ED50=4.6 mg/L）.
基金Hebei Province Supporting Natural Science Fund(No.06276470)
文摘Objective To establish a rapid method for detecting acetylbritannilactone （ABL） by online sweeping-micellar electrokinetic chromatography （MEKC） and to elevate the sensitivity of the detection. Methods The combination of online sweeping technique with MEKC was used to determine the content of ABL in the extract of Inula britannica in plasma of rats. Results ABL was completely separated within 15 min in running buffer and sample buffer. The optimal conditions were as follows： on uncoated fused quartz silica capillary, with separation voltage of 23 kV, capillary temperature of 25 oC, and detection wavelength of 195 nm. The regression equations revealed good linear relationships between the peak area and concentration of ABL （r = 0.998）, with the detection limits of 0.005-0.15 mg/mL. The relative standard deviations of migration time and peak areas for intra- and inter-batch were 〈 2.45% and 〈 2.26%, respectively. The recovery rate of this method was 96.3~97.2%. Conclusion This method provides some advantages in separation speed, testing sensitivity, and operating convenience, with low sample and reagent consumption. The online sweeping-MEKC is an effective method for pharmacokinetic study and analysis on tracing biological samples.
