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超声辅助离子液体—反相液相色谱法测定赤芍中齐墩果酸和芍药苷的含量(1)
http://www.100md.com 2015年2月1日 中国中药杂志 2015年第3期
     [摘要]建立以4种离子液体为萃取剂,结合超声辅助萃取,利用高效液相色谱法测定赤芍中齐墩果酸和芍药苷的方法。采用Purospher star RP-C18柱(4.6 mm×250 mm, 5 μm ),测定齐墩果酸含量时以乙腈-水(90∶10)为流动相,流速1.0 mL·min-1,紫外检测波长210 nm,柱温室温;测量芍药苷含量时以乙腈-水(18∶82)为流动相,流速1.0 mL·min-1,紫外检测波长250 nm,柱温室温。结果显示,齐墩果酸的最佳萃取剂为0.6 mol·L-1的Br甲醇溶液,最佳固液比为1∶80(g·mL-1),进样量在0.24~3.76 μg呈良好的线性关系(r=0.999 9),平均回收率为97.20%;芍药苷的最佳萃取剂为0.6 mol·L-1的[C4MIM]PF6甲醇溶液,最佳固液比为1∶130(g·mL-1),进样量在0.42~4.20 μg呈线性关系(r=1.000),平均回收率为98.84%。该方法操作简便可靠,重复性好,对赤芍进行离子液体微萃取研究有重要意义。
, 百拇医药
    [关键词]赤芍; 芍药苷; 齐墩果酸; 离子液体; HPLC

    [收稿日期]2014-10-03

    [基金项目]河南省青年骨干教师计划项目(教高[2012]704号);河南省科技厅基础前沿计划项目(142300410123,132300410255);河南大学研究生教育综合改革项目(Y1411008);河南大学大学生创新创业训练计划项目(14NA016)

    [通信作者]*郭秀春,Tel:(0371)23880680,E-mail:guoxiuchun@henu.edu.cnDetermination of oleanic acid and paeoniflorin in Paeonia lactiflora by

    ultrasound-assisted ionic liquid-reversed phase liquid chromatography
, 百拇医药
    LIU Wei1, LI Dong-dong1, YANG Hong-shuai1, CHEN Yuan-yuan1, WEI Jin-feng1,2, KANG Wen-yi1, GUO Xiu-chun1*

    (1.Institute of Natural Products, He′nan University, Kaifeng 475004, China;

    2.Minsheng College, He′nan University, Kaifeng 475004, China)

    [Abstract]Four kinds of ionic liquids Br, BF4, PF6, [HMIM]PF6 were used to analyze the content of oleanic acid and paeoniflorin in Paeonia lactiflora with ultrasonic-assisted extraction coupled with HPLC. The chromatographic column, Purospher star RP-C18 (4.6 mm×250 mm, 5 μm), was used. Acetonitrile and water (90∶10) as mobile phase was used to determine the content of oleanic acid with a gradient elution and flow rate at 1.00 mL·min-1, detection wavelength at 210 nm, chromatographic column temperature at room temperature. Paeoniflorin content was determined using acetonitrile and water (18∶82) as mobile phase with a gradient elution and flow rate at 1.00 mL·min-1, detection wavelength at 250 nm, the chromatographic column temperature at room temperature. The result show that oleanic acid has the highest extraction yield when the conditions are solid-liquid ratio of 1∶80 (g·mL-1), and the Br methanol solution concentration of 0.6 mol·L-1. Under the optimal extraction conditions, the content of oleanic acid from 0.24 to 3.76 μg showed a good linearity (r = 0.999 9), the average recovery was 97.20%. Paeoniflorin has the highest extraction yield when the conditions are solid-liquid ratio of 1∶130 (g·mL-1), and the [C4MIM]PF6 methanol solution concentration of 0.6 mol·L-1. Under the optimal extraction conditions, paeoniflorin content from 0.42 to 4.20 μg showed a good linearity (r=1.000), the average recovery was 98.84%. This method is simple and reliable, its repeatability is also very good. It has important significance in the study P. lactiflora of ionic liquid microextraction., 百拇医药(刘微 李冬冬 杨洪帅 陈圆圆 魏金凤 康文艺 郭秀春)
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