UPLC-PDA-ELSD测定贵州山银花中绿原酸、灰毡毛忍冬皂苷乙和川续断皂苷乙的含量  

Simultaneous Determination of Chlorogenic Aicd,Macranthoidin B and Dipsacoside B in Lonicerae Flos by UPLC with PDA and ELSD

作　　者：赵留存[1] 叶世芸[1] 杨春[2] 林昌虎[3] 赵巡 郭云[1] 

机构地区：[1]贵阳中医学院,贵阳550002 [2]贵州理工学院,贵阳550003 [3]贵州科学院,贵阳550001

出　　处：《中国实验方剂学杂志》2015年第7期64-67,共4页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：贵州省中药现代化重大专项[黔科合重大专项字(2012)6010号]

摘　　要：目的：建立超高效液相色谱-紫外检测器-蒸发光检测器联用（UPLC-PDA-ELSD）同时测定山银花中绿原酸、灰毡毛忍冬皂苷乙和川续断皂苷乙含量的方法,并考察贵州地区山银花的质量。方法：采用ACQUITY UPLC BEH C18色谱柱（2.1mm×100 mm,1.7μm）,流动相乙腈（A）-0.4%乙酸水（B）,梯度洗脱（0-2 min,7%A;2-2.3 min,7%-28%A;2.3-10 min,28%A;10-10.5 min,28%-7%A）,梯度流速（0-2 min,0.35 mL·min^-1;2-2.3 min,0.35-0.25 mL·min^-1;2.3-2.6 min,0.25-0.15 mL·min^-1;2.6-2.8 min,0.15-0.1 mL·min^-1;2.8-4 min,0.1-0.2 mL·min^-1;4-4.3 min,0.2-0.3 mL·min^-1;4.3-4.5 min,0.3-0.35 mL·min^-1;4.5-10.5 min,0.35 mL·min^-1）,PDA（紫外检测器）检测绿原酸（330 nm）;ELSD（蒸发光散射检测器）检测灰毡毛忍冬皂苷乙和川续断皂苷乙,漂移管温度60℃,喷雾器温度48℃,气体压力20 psi,色谱柱温度50℃。结果：绿原酸、灰毡毛忍冬皂苷乙和川续断皂苷乙3种成分分别在0.304 5-1.522 5（R^2=0.999 4）,0.449-1.436 8（R^2=0.999 3）,0.044 6-0.223μg（R^2=0.999 4）呈良好的线性关系。结论：该方法能方便准确的测定贵州山银花中绿原酸、灰毡毛忍冬皂苷乙和川续断皂苷乙的含量,并能有效缩短测量时间和节省试剂。此方法适用于测定考察贵州地区山银花的质量。Objective： To establish a method for determination of chlorogenic acid, galuteolin and dipsaeoside B in Lonicerae Flos using Ultra Performance Liquid Chromatography, and inspect the quality of the Lonicerae Flos in Guizhou. Method： ACQUITY UPLC BEH C18 （2. 1 mm ×100 mm,1.7μm） column was adopted. Two solution were acetonitrile and water containing 0.4% acetic acid, with gradient elution of （0-2 min, 7% A; 2-2.3 min, 7% -28% A; 2.3-10 min, 28% A; 10-10.5 min, 28% -7% A） , and velocity gradient （0- 2 min, 0.35 mL·min^-1; 2-2.3 rain, 0.35-0.25 mL·min^-1; 2. 3-2.6 min, 0.25-0. 15 mL·min^-1; 2.6-2.8 min, 0. 15-0. 1 mL·min^-1 ; 4.3-4.5 min, ; 2. 8-4 min, 0. 1-0.2 mL·min^-1; 4-4.3 min, 0.2-0.3 mL ·min^-1 ,0. 3-0. 35 mL·min^-1; 4.5-10.5 min, 0.35 mL ·min^-1 ）. The PDA detection wavelength was 330 nm for chlorogenic aicd. The ELSD detection was for macranthoidin B and dipsacoside B. The temperature of drift tube was maintained at 60 ℃ , the temperature of nebulizer was 48 ℃ , with the nitrogen flow rate of 20 psi, and the column temperature was maintained at 50 ℃. Result： The linear response ranges of chlorogenic acid, galuteolin and dipsaeoside B were0.3045-1.522 5 （R^2 =0.999 4）, 0.449-1.436 8 （R^2 =0.9993）, 0.044 6-0. 223 μg （R^2 = 0. 999 chlorogenic a saves reagent 4） cid , respectively. Conclusion： The method is convenient and accurate to determine the content of , macranthoidin B and dipsacoside B in Lonicerae Flos , and can shorten the effectively. The established method has used to measure quality of the Lonicerae measuring time and Flos in Guizhou.

关 键 词：山银花 绿原酸 灰毡毛忍冬皂苷乙 川续断皂苷乙 

分 类 号：R284.1[医药卫生—中药学]