在线固相萃取法结合电雾式检测器测定黄芪及其复方中黄芪甲苷的含量  

Determination of Astragaloside IV in Radix Astragli and Its Preparations by Online SPE-Liquid Chromatography with Charged Aerosol Detector

作　　者：李效宽[1] 张艳海 冯天辉 杨艳羚[1] 金燕 

机构地区：[1]中南民族大学药学院,武汉430074 [2]赛默飞世尔科技(中国)有限公司,上海201205

出　　处：《分析化学》2014年第12期1791-1796,共6页Chinese Journal of Analytical Chemistry

摘　　要：采用在线固相萃取高效液相色谱法,结合电雾式检测器,建立了快速测定黄芪及其复方中黄芪甲苷的方法。采用Acclaim Polar AdvantageⅡC18（50 mm＆#215;4.6 mm,3μm）为在线净化柱,以双三元液相色谱的右泵作为上样净化泵,甲醇-水为流动相,梯度洗脱,进行富集和净化；采用Acclaim C18（150 mm＆#215;4.6 mm,5μm）为分析柱,以双三元液相色谱的左泵作为分析泵,乙腈-水作为流动相,等度洗脱,流速为1.0 mL/min,采用中心切割的方式将目标物从在线净化柱转移至分析柱中。电雾式检测器（ CAD）的雾化器温度为30℃；氮气压力为241.3 kPa。黄芪甲苷在药材及复方基质中获得较好分离,黄芪甲苷在4.0～80 mg/L范围内,相关系数r=0.9998,平均回收率为97.6％。实验表明,本方法快速、简便,专属性、重现性较好,测定结果可靠,可应用于黄芪及其复方中黄芪甲苷含量的检测。A novel method for quantification of astragaloside online SPE liquid chromatography coupled with corona charged IV in Radix Astragli was developed by using aerosol detection（CAD）. The sample solutionwas loaded into Acclaim Polar Advantage Ⅱ C18（50 mm×4.6 mm, 3 μm） which was selected as online SPE column. Then the cleaning process was done by using the Right one of dual gradient pumps with Methanol- water as mobile phase. Acclaim C18 （150 mm×4.6 mm, 5 μm） was selected as analytical column with acetonitrile-water as mobile phase at a flow rate of 1.0 mL/min. The eluate containing the target from SPE eolumn was transferred into the analytical column by heart-cutting mode. The temperature of nebulizer of corona CAD was set at 30 % and the nitrogen pressure was 241.3 kPa. The baseline separation of astragaloside IV from matrix components has been achieved. There was a good linear correlation in the range of 4.0-80 mg/L for astragaloside IV and the correlation coefficient was 0. 9998. The standard addition average recovery of astragaloside IV in Radix Astragli was 97.6%. Astragli and its preparations can be quantified rapidly and It has been validated that astragaloside IV in Radix accurately with this method.

关 键 词：黄芪甲苷 在线固相萃取 电雾式检测器 双三元液相色谱 

分 类 号：O657.72[理学—分析化学] R284[理学—化学]