摘要
目的:通过高效液相指纹图的检测方法测试不同批次参苓白术散中人参皂苷的含量。方法:进样量为10μL,采用250 mm×4. 6 mm,5μm的色谱柱(Thermo ODS-HYPERSIL柱),选择流动相的条件是在A流动相乙腈和B流动相水中以1m L/min的流速开展实验,检测波长为203 nm,柱温为30℃,根据高效液相(HPLC)(Agilengt-1100高效液相色谱仪)指纹图谱的梯度洗脱程序进行试验,并在Agilengt-1100色谱工作站上进行指纹图谱分析。分别对HPLC方法学的严谨性进行检测,包括专属性试验、精密度试验、稳定性试验、重复性试验、线性回归试验、加样回收率试验等逐步建立方法的科学性;而后进一步采用HPLC对参苓白术散中人参皂苷的含量进行具体的检测和记录。结果:1) HPLC的专属性试验结果显示人参皂苷Rg1、Re及Rb1均有良好的专属性。2)人参皂苷Rg1的线性回归方程是Y=352. 681 19X+6. 738 50;人参皂苷Re的线性回归方程是Y=292. 610 86X+3. 703 23;人参皂苷的线性回归方程是Rb1Y=254. 203 21X+4. 564 71;其相关系数均> 0. 999,结果显示人参皂苷线性关系良好。3)精密度试验结果显示人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1峰面积的RSD在0. 22%～0. 29%;稳定性试验结果显示人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1峰面积的RSD在0. 06%～1. 83%;重复性试验结果显示人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1总量的含量平均值为9. 86 mg,RSD 2. 5%表明HPLC的精密度、稳定性和重复性均良好。4)结果显示人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1的加样回收率平均值和RSD分别为95. 7%、105. 7%、100. 4%,3. 3%、4. 8%、3. 1%,表明均HPLC测定参苓白术散加样回收率良好。5)不同批次参苓白术散中人参皂苷总的含量存在较大差别。结论:高效液相指纹图谱检测参苓白术散的操作方法较为简便,其专属性、灵敏度和重复性均较好,而不同批次参苓白术散中人参皂苷总的含量存在
Objective ：To establish a method for the determination of ginsenosides in Shenling Baizhu powder by high performance liquid chromatography fingerprint, so as to improve the quality control of Shenling Baizhu powder. Methods ： Chromatographic conditions ： ThermoODS-HYPERSIL column （250 mm × 4. 6 mm ,5 micron）, mobile phase （ flow rate ： 1 mL/min） ： aeetonitrile ：water, injection volume ： 10 mieroL, colunm temperature ： 30℃ , detection wavelength ： 203 nm. The standard curve of ginsenoside reference substance series concentration ,blank reference solution were prepared. Shenling Baizhu powder detection solution were carried out on the tested samples, and the liquid ehromatogram was processed and analyzed by Agilengt-1100 chromatographic workstation, specific test,precision test,stability test, repeatability test,linear regression test and sample recovery test were done accorded to the procedures, the chromatographic conditions of the high performance liquid chromatography were validated methodologically. Six bat- ehes of Shenling Baizhu Powder were processed and prepared for inspected solution. The content of ginsenosides in the samples were determined by the above-mentioned chromatographic conditions. Results ： 1 ） HPLC specific test ： ginsenoside Rgl, Re and Rbl have good specificity. 2） Linear regression equation of ginsenoside Rgl was Y = 352. 681 19X ＋6. 738 50; ginsenoside Re linear regression equation was Y =292. 610 86X ＋ 3. 703 23; ginsenoside linear regression equation was RblY =254. 203 21X ＋4. 564 71 ; the correlation coefficients all exceeded 0. 999, and had good linear relationship. 3） Precision test：RSD of peak area of ginsen- oside Rgl, ginsenoside Re and ginsenoside Rbl ranged from 0. 22% to 0. 29%. Stability test showed that RSD of peak area of gin- senoside Rgl, ginsenoside Re and ginsenoside Rbl ranged from 0. 06% to 1.83 %. 4） Repeatability test ： ginsenosition test ： ginsen- oside Rgl, ginsenoside Re, ginsenoside Rbl The average content of t
作者
王雪梅
李艳娇
宋燕青
Wang Xuemei;Li Yanjiao;Song Chunyan(Department of pharmacy,The First Hospital of Jilin University,Changchun 130000,China)
出处
《世界中医药》
CAS
2018年第11期2876-2879,2883,共5页
World Chinese Medicine
基金
国家自然科学基金项目(81274036)
关键词
参苓白术散
高效液相
指纹图谱
人参皂苷
人参皂苷Rg1
人参皂苷RE
人参皂苷RB1
含量测定
Shenling Baizhu powder
High performance liquid chromatography
Fingerprint
Ginsenoside
Ginsenoside Rg1
Ginsenoside Re
ginsenoside Rb1
Content determination
