分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
12期
1791-1796
,共6页
李效宽%张艳海%冯天辉%杨艳羚%金燕
李效寬%張豔海%馮天輝%楊豔羚%金燕
리효관%장염해%풍천휘%양염령%금연
黄芪甲苷%在线固相萃取%电雾式检测器%双三元液相色谱
黃芪甲苷%在線固相萃取%電霧式檢測器%雙三元液相色譜
황기갑감%재선고상췌취%전무식검측기%쌍삼원액상색보
Astragaloside IV,Online solid phase extraction%Corona chard aerosol detection%Dual liquid chromatography
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×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×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。
採用在線固相萃取高效液相色譜法,結閤電霧式檢測器,建立瞭快速測定黃芪及其複方中黃芪甲苷的方法。採用Acclaim Polar AdvantageⅡC18(50 mm×4.6 mm,3μm)為在線淨化柱,以雙三元液相色譜的右泵作為上樣淨化泵,甲醇-水為流動相,梯度洗脫,進行富集和淨化;採用Acclaim C18(150 mm×4.6 mm,5μm)為分析柱,以雙三元液相色譜的左泵作為分析泵,乙腈-水作為流動相,等度洗脫,流速為1.0 mL/min,採用中心切割的方式將目標物從在線淨化柱轉移至分析柱中。電霧式檢測器( CAD)的霧化器溫度為30℃;氮氣壓力為241.3 kPa。黃芪甲苷在藥材及複方基質中穫得較好分離,黃芪甲苷在4.0~80 mg/L範圍內,相關繫數r=0.9998,平均迴收率為97.6%。實驗錶明,本方法快速、簡便,專屬性、重現性較好,測定結果可靠,可應用于黃芪及其複方中黃芪甲苷含量的檢測。
채용재선고상췌취고효액상색보법,결합전무식검측기,건립료쾌속측정황기급기복방중황기갑감적방법。채용Acclaim Polar AdvantageⅡC18(50 mm×4.6 mm,3μm)위재선정화주,이쌍삼원액상색보적우빙작위상양정화빙,갑순-수위류동상,제도세탈,진행부집화정화;채용Acclaim C18(150 mm×4.6 mm,5μm)위분석주,이쌍삼원액상색보적좌빙작위분석빙,을정-수작위류동상,등도세탈,류속위1.0 mL/min,채용중심절할적방식장목표물종재선정화주전이지분석주중。전무식검측기( CAD)적무화기온도위30℃;담기압력위241.3 kPa。황기갑감재약재급복방기질중획득교호분리,황기갑감재4.0~80 mg/L범위내,상관계수r=0.9998,평균회수솔위97.6%。실험표명,본방법쾌속、간편,전속성、중현성교호,측정결과가고,가응용우황기급기복방중황기갑감함량적검측。
A novel method for quantification of astragaloside IV in Radix Astragli was developed by using online SPE liquid chromatography coupled with corona charged aerosol detection( CAD) . The sample solution <br> was loaded into Acclaim Polar AdvantageⅡC18(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 column 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%. It has been validated that astragaloside IV in Radix Astragli and its preparations can be quantified rapidly and accurately with this method.