一测多评法同时测定蒙药沙黄清疫片中9个成分的含量  

Simultaneous Determination of Nine Constituents in Shahuang Qingyi Tablets by QAMS

作　　者：徐秀娟 杨立国 吴凤娇 萨其拉吐 那布其 包书茵[3] 奥·乌力吉 包晓华[1,2] 佟海英 XU Xiujuan;YANG Liguo;WU Fengjiao;SA Qilatu;NA Buqi;BAO Shuyin;AO Wuliji;BAO Xiaohua;TONG Haiying(Mongolian Medicine Engineering Technology Institute of Inner Mongolia,Tongliao 028000,China;Mongolian Medical College,Inner Mongolia Minzu University,Tongliao 028000,China;School of Medicine,Inner Mongolia Minzu University,Tongliao 028000,China;School of Traditional Chinese Medicine,Beijing University of Chinese Medicine,Beijing 100029,China)

机构地区：[1]内蒙古蒙医药工程技术研究院,通辽028000 [2]内蒙古民族大学蒙医药学院,通辽028000 [3]内蒙古民族大学医学院,通辽028000 [4]北京中医药大学中医学院,北京100029

出　　处：《世界中医药》2025年第4期547-552,共6页World Chinese Medicine

基　　金：国家重点研发计划项目(2018YFC1708200);内蒙古自治区科技计划项目(2020GG0233)。

摘　　要：目的:建立一测多评法(QAMS)同时测定蒙药沙黄清疫片中荭草苷、毛蕊异黄酮葡萄糖苷、牡荆素、胡黄连苷Ⅱ、水仙苷、1,5-二咖啡酰奎宁酸、香叶木素、异鼠李素和芒柄花素9个成分的含量。方法:采用高效液相色谱(HPLC)法,以Agilent Eclipse Plus C_(18)柱(250 mm×4.6 mm,5μm),流动相乙腈-甲醇-0.4%磷酸水溶液,流速1.0 mL/min进行梯度洗脱,柱温30℃,检测波长245 nm;以1,5-二咖啡酰奎宁酸为内参物,分别测定内参物与荭草苷、毛蕊异黄酮葡萄糖苷、牡荆素、胡黄连苷Ⅱ、水仙苷、香叶木素、异鼠李素和芒柄花素的相对校正因子(fs/i),测定沙黄清疫片中9个成分的含量。考察不同色谱柱和色谱仪中9个成分相对校正因子的稳定性和耐用性,比较QAMS和外标法(ESM)测定结果的差异。结果:蒙药沙黄清疫片中荭草苷、毛蕊异黄酮葡萄糖苷、牡荆素、胡黄连苷Ⅱ、水仙苷、香叶木素、异鼠李素和芒柄花素8种成分的fs/i分别为1.2281、1.1296、0.7507、0.3521、0.8809、1.1153、0.6251、4.1604;在3种HPLC色谱仪及3个不同品牌C_(18)色谱柱的相对标准偏差(RSD)范围为0.76%~2.78%、在不同柱温(25℃、30℃、35、40℃)RSD范围为0.70%~1.76%,不同体积流量(0.6 mL/min、0.8 mL/min、1.0 mL/min、1.2 mL/min)下的RSD范围为0.34%~2.08%,表明相对校正因子的耐用性良好。QAMS与ESM含量测定结果的相对误差(RE)值均小于2%,无显著差异。结论:以1,5-二咖啡酰奎宁酸为内参物建立的一测多评法高效、准确、可行,能有效地测定沙黄清疫片9个成分的含量,可用于其质量评价。Objective:To establish a quantitative analysis of multi-components by a single marker(QAMS)method for the simultaneous determination of nine components in Mongolian medicine Shahuang Qingyi Tablets,including orientin,calycosin-7-O-β-D-glucoside,vitexin,picrosideⅡ,narcissoside,1,5-dicaffeoylquinic acid,diosmetin,isorhamnetin,and formononetin.Methods:High-performance liquid chromatography(HPLC)was employed using an Agilent Eclipse Plus C_(18) column(250 mm×4.6 mm,5μm).The mobile phase consisted of acetonitrile-methanol-0.4%phosphoric acid aqueous solution with a gradient elution at a flow rate of 1.0 mL/min.The column temperature was set at 30℃,and the detection wavelength was 245 nm.Using 1,5-dicaffeoylquinic acid as the internal reference,the relative correction factors(f s/i)of orientin,calycosin-7-O-β-D-glucoside,vitexin,picrosideⅡ,narcissoside,diosmetin,isorhamnetin,and formononetin were determined to quantify these nine components in Shahuang Qingyi Tablets.The stability and robustness of the relative correction factors were evaluated across different chromatographic columns and instruments.The results obtained using the QAMS method were compared with those obtained using the external standard method(ESM).Results:The relative correction factors for the eight components in Shahuang Qingyi Tablets were determined as follows:orientin(1.2281),calycosin-7-O-β-D-glucoside(1.1296),vitexin(0.7507),picrosideⅡ(0.3521),narcissoside(0.8809),diosmetin(1.1153),isorhamnetin(0.6251),and formononetin(4.1604).The relative standard deviations(RSDs)of the correction factors across three different HPLC instruments and three different C_(18) columns ranged from 0.76%to 2.78%.Under different column temperatures(25℃,30℃,35℃,40℃),the RSDs ranged from 0.70%to 1.76%,and under different flow rates(0.6,0.8,1.0,and 1.2 mL/min),the RSDs ranged from 0.34%to 2.08%,indicating good robustness of the relative correction factors.The relative errors(REs)between the QAMS and ESM results were all below 2%,showing no significant

关 键 词：蒙药沙黄清疫片 一测多评法 1 5-二咖啡酰奎宁酸 荭草苷 毛蕊异黄酮葡萄糖苷 牡荆素 胡黄连苷Ⅱ 水仙苷 

分 类 号：R29[医药卫生—民族医学]