快速溶剂萃取-超高效液相色谱法测定稳心颗粒中皂苷类成分  

Determination of saponins in Wenxin granules by ASE- UPLC

作　　者：李启艳[1,2] 王荣梅[3] 

机构地区：[1]山东中医药大学,济南250355 [2]山东省食品药品检验所,济南250101 [3]山东大学第二医院,济南250033

出　　处：《药物分析杂志》2015年第3期528-531,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：建立快速溶剂萃取-超高效液相色谱法,用以测定稳心颗粒中三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1的含量。方法：利用乙醚脱脂,水饱和正丁醇提取制剂中皂苷;采用Agilent Eclipse Pluse C18色谱柱（2.1 mm×50 mm,1.8μm）分离,以乙腈（A）-水（B）为流动相,梯度洗脱（0-10 min,81%B;10-17 min,81%B→45%B;17-18 min,45%B→81%B;18-25 min,81%B）,流速0.3 m L·min-1,柱温25℃,检测波长203 nm。与普通提取方法比较,提取时间由14 h缩短到25 min,大幅度提高样品处理效率。结果：三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1进样量分别在0.084-0.84μg（r=0.999 9）、0.201 6-2.016μg（r=0.999 8）、0.208 4-2.084μg（r=0.999 9）范围内呈良好线性关系,平均加样回收率（n=6）分别为98.4%（RSD=1.1%）、98.2%（RSD=0.47%）、97.9%（RSD=1.3%）。样品中总皂苷含量为2.65 mg·g-1,与中国药典方法测定结果（2.63 mg·g-1）基本一致。采用快速溶剂萃取-超高效液相色谱法,测定时间比普通的高效液相色谱法缩短了约40 min。结论：该方法经方法学验证,适用于稳心颗粒中皂苷类成分的快速测定。Objective： To develop a novel method for the rapid extraction and determination of notoginsenoside R1,ginsenoside Rg1 and ginsenoside Rb1 in Wenxin granules by accelerated solvent extraction（ ASE） coupled with ultra-performance liquid chromatography（ UPLC）. Methods： Ether was used to remove the lipid ingredients and water- saturated butanol solution was adopted to extract the saponins. The analysis was performed on an Agilent Eclipse Pluse C18column（ 2. 1 mm × 50 mm,1. 8 μm）,the mobile phase consisted of acetonitrile（ A） and water（ B） with gradient program（ 0- 10 min,81% B; 10- 17 min,81% B→45% B; 17- 18 min,45% B→81% B; 18- 25 min,81% B）. The detection wavelength was 203 nm and the column temperature was set at 25 ℃. In comparison with traditional method,ASE reduced the extraction time from 14 h to 25 min and substantially increased processing efficiency. Results： The linearity was achieved in the range of 0. 084- 0. 84 μg（ r = 0. 999 9） for notoginsenoside R1,0. 201 6-2. 016 μg（ r = 0. 999 8） for ginsenoside Rg1 and 0. 208 4- 2. 084 μg（ r = 0. 999 9） for ginsenoside Rb1. The average recoveries（ n = 6） for each were 98. 4 %（ RSD = 1. 1 %）,98. 2 %（ RSD = 0. 47 %） and 97. 9 %（ RSD =1. 3 %）. The content of saponins was 2. 65 mg·g- 1essentially in agreement with Chinese pharmacopoeia method（ 2. 63 mg·g- 1）. The determination time was 40 minutes shorter by UPLC than by HPLC Conclusion： The method was suitable for the determination of saponins in Wenxin granules.

关 键 词：中药快速分析 稳心颗粒 三七皂苷R1 人参皂苷Rg1 人参皂苷RB1 快速溶剂萃取(ASE) 超高效液相色谱(UPLC) 

分 类 号：R917[医药卫生—药物分析学]