一测多评法同时测定大黄药材中8个结合型蒽醌含量的系统研究  

Systematic study on simultaneous determination of eight anthraquinone glycosides in Rhei Radix et Rhizoma by QAMS

作　　者：冯亚茹 周荣荣 耿佳乐 黄志永 王璐瑶 窦志华[1,2,3] FENG Ya-ru;ZHOU Rong-rong;GENG Jia-le;HUANG Zhi-yong;WANG Lu-yao;DOU Zhi-hua(Affiliated Nantong Hospital 3 of Nantong University,Nantong 226006,China;Nantong University,Nantong 226019,China;Nanjing University of Chinese Medicine,Nanjing 210023,China)

机构地区：[1]南通大学附属南通第三医院,南通226006 [2]南通大学,南通226019 [3]南京中医药大学,南京210023

出　　处：《药物分析杂志》2022年第11期1884-1894,共11页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省重点研发计划(社会发展)项目(BE2018674);江苏省中医药科技计划项目(YB201836)。

摘　　要：目的:建立分别以其中任何1个结合型蒽醌为内参物均可用于测定大黄药材中8个结合型蒽醌的一测多评法(QAMS法)。方法:采用高效液相色谱法,色谱柱为Symmetry C18(250 mm×4.6 mm,5μm),以甲醇(A)-0.1%磷酸水(B)为流动相进行梯度洗脱,流速为1.0 mL·min^(-1),柱温为30℃,检测波长为280 nm。分别以芦荟大黄素-8-O-葡萄糖苷、大黄酸-8-O-葡萄糖苷、大黄素-1-O-葡萄糖苷、大黄酚-1-O-葡萄糖苷、大黄酚-8-O-葡萄糖苷、芦荟大黄素-3-羟甲基-O-葡萄糖苷、大黄素-8-O-葡萄糖苷、大黄素甲醚-8-O-葡萄糖苷为内参物,采用多点校正法,建立另外7个待测成分与内参物的相对校正因子(RCFs),计算待测成分与内参物色谱峰的相对保留时间(RRTs)。采用RCFs计算分别以其中1个成分为内参物时28批大黄药材中另外7个待测成分的含量,以差异百分比(PD)为参数,与外标法(ESM)测定结果进行比较,验证QAMS的准确性。结果:分别以芦荟大黄素-8-O-葡萄糖苷、大黄酸-8-O-葡萄糖苷、大黄素-1-O-葡萄糖苷、大黄酚-1-O-葡萄糖苷、大黄酚-8-O-葡萄糖苷、芦荟大黄素-3-羟甲基-O-葡萄糖苷、大黄素-8-O-葡萄糖苷、大黄素甲醚-8-O-葡萄糖苷为内参物时,另外7个待测成分与内参物的RCFs分别为1.435、0.624、1.206、0.849、1.718、0.563、0.549,0.697、0.435、0.841、0.592、1.197、0.392、0.383,1.603、2.3、1.932、1.36、2.753、0.897、0.88,0.83、1.191、0.518、0.704、1.425、0.464、0.455,1.178、1.691、0.736、1.421、2.024、0.663、0.647,0.582、0.835、0.363、0.702、0.494、0.328、0.32,1.788、2.566、1.117、2.157、1.518、3.072、0.982和1.822、2.616、1.137、2.197、1.547、3.13、1.025,RRTs分别为1.207、1.47、1.68、1.719、1.763、1.768、2.015,0.829、1.218、1.393、1.425、1.461、1.466、1.671,0.681、0.821、1.143、1.169、1.199、1.203、1.371,0.596、0.719、0.876、1.023、1.049、1.053、1.2,0.583、0.703、0.856、0.977、1.026、1.029、1.173,0.568Objective:To establish a quantitative analysis of multi-components by single marker(QAMS)method for the determination of eight anthraquinone glycosides in Rhei Radix et Rhizoma when any one of them was chosen as the internal reference substance.Methods:HPLC method was developed on a Symmetry C18(250 mm×4.6 mm,5μm)column with methanol(A)-0.1%phosphoric acid(B)as mobile phase for a gradient elution.The flow rate was set at 1.0 mL·min^(-1),the temperature maintained at 30℃,and the detection wavelength was set at 280 nm.Aloe emodin-8-O-glucoside,rhein-8-O-glucoside,emodin-1-O-glucoside,chrysophanol-1-O-glucoside,chrysophanol-8-O-glucoside,aloe emodin-3-CH2-O-glucoside,emodin-8-O-glucoside,and physcion-8-O-glucoside was chosen as the internal reference substance,respectively,the relative correction factors(RCFs)of other seven components to be measured to the internal reference substances were established by multi-point correction method,and the relative retention time(RRTs)of the chromatographic peaks of components to be measured to the ones of the internal reference substances were calculated,respectively.The contents of other seven components to be measured in 28 batches of Rhei Radix et Rhizoma were calculated by RCFs when one of the eight components was used as the internal reference substance respectively,and the percentage difference(PD)was used as a parameter to compare the results with that of external standard method(ESM)to verify the accuracy of QAMS.Results:When aloe emodin-8-O-glucoside,rhein-8-O-glucoside,emodin-1-O-glucoside,chrysophanol-1-O-glucoside,chrysophanol-8-O-glucoside,aloe emodin-3-CH2-O-glucoside,emodin-8-O-glucoside,and physcion-8-O-glucoside was used as internal reference substance respectively,the RCFs of the other seven components to be measured to the internal reference substances were(1.435,0.624,1.206,0.849,1.718,0.563,0.549),(0.697,0.435,0.841,0.592,1.197,0.392,0.383),(1.603,2.3,1.932,1.36,2.753,0.897,0.88),(0.83,1.191,0.518,0.704,1.425,0.464,0.455),(1.178,1.691,0.736,1.421,2.024,

关 键 词：大黄 结合型蒽醌 芦荟大黄素-8-O-葡萄糖苷 大黄酸-8-O-葡萄糖苷 大黄素-1-O-葡萄糖苷 大黄酚-1-O-葡萄糖苷 大黄酚-8-O-葡萄糖苷 芦荟大黄素-3-羟甲基-O-葡萄糖苷 大黄素-8-O-葡萄糖苷 大黄素甲醚-8-O-葡萄糖苷 一测多评 

分 类 号：R917[医药卫生—药物分析学]