HPLC-DAD-ELSD法同时测定消栓通络片中10种成分的含量  

Simultaneous Determination of 10 Constituents in Xiaoshuan Tongluo Tablets by HPLC-DAD-ELSD

作　　者：马靖 袁兴君 杨雪姣 杨溢 Ma Jing;Yuan Xingjun;Yang Xuejiao;Yang Yi(The Third People’s Hospital of Beilun District in Ningbo City,Zhejiang Ningbo 315801,China;Jinhua Hospital of TCM)

机构地区：[1]宁波市北仑区第三人民医院,浙江宁波315801 [2]金华市中医医院

出　　处：《中国药师》2020年第10期2057-2061,共5页China Pharmacist

摘　　要：目的:同时测定消栓通络片中10种成分的含量。方法:采用HPLC-DAD-ELSD法,色谱柱:Waters Symmetry C18(250 mm×4.6 mm,5μm);流动相:乙腈(A)-0.1%磷酸溶液(B),梯度洗脱;流速:1.0 ml·min^-1;柱温:30℃;毛蕊异黄酮葡萄糖苷、阿魏酸、芦丁、金丝桃苷、丹酚酸B、肉桂酸测定的DAD检测器参数:检测波长:260 nm(毛蕊异黄酮葡萄糖苷)、316 nm(阿魏酸)、360 nm(芦丁和金丝桃苷)、285 nm(丹酚酸B和肉桂酸);三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、黄芪甲苷测定的ELSD检测器参数:漂移管温度40℃;气体流量:1.5 L·min-1。结果:毛蕊异黄酮葡萄糖苷、阿魏酸、芦丁、金丝桃苷、丹酚酸B、肉桂酸、三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、黄芪甲苷分别在为0.268~5.350,0.232~4.650,5.016~100.32,0.606~12.128,4.924~98.480,8.208~164.160,5.068~101.360,14.008~280.160,12.392~247.840,1.029~20.576μg·ml-1(r为0.9995~0.9998)浓度范围内呈良好的线性关系;平均加样回收率分别为94.9%,95.9%,96.9%,101.6%,97.3%,98.2%,99.3%,99.9%,97.0%,94.8%,RSD分别为1.1%,1.1%,0.2%,1.0%,0.7%,1.1%,0.4%,0.4%,0.5%,1.2%(n=6)。结论:本文建立测定方法专属性强,重复性好,灵敏度高,适用于消栓通络片中10种成分的测定,为完善消栓通络片质量评价标准提供依据。Objective:To establish a quantitative method for the determination of 10 constituents in Xiaoshuan Tongluo tablets simultaneously.Methods:The HPLC-DAD-ELSD method was adopted on a Waters Symmetry C18 column(250 mm×4.6 mm,5μm).The mobile phase consisted of acetonitrile(A)-0.1%aqueous phosphoric acid(B)with gradient elution at the flow rate of 1.0 ml·min-1.The column temperature was 30℃.The determination of glucoside,ferulic acid,rutin,hyperoside,salvianolic acid B and cinnamic acid was detected by a DAD detector at 260nm(calycosin7-O-β-D-glycoside),316 nm(ferulic acid),360 nm(rutin and hyperoside)and 285 nm(salvianolic acid B and cinnamic acid).The determination conditions of notoginsenoside R1,ginsenoside Rg1,ginsenoside Rb1 and astragaloside IV by ELSD were as follows:the temperature of drift tube was 40℃and the gas flow rate was 1.5 L·min^-1.Results:The range of linear correlation of calycosin7-O-β-D-glycoside,ferulic acid,rutin,hyperoside,salvianolic acid B,cinnamic acid,notoginsenoside R1,ginsenoside Rg1,ginsenoside Rb1 and astragaloside IV was 0.268-5.350,0.232-4.650,5.016-100.32,0.606-12.128,4.924-98.480,8.208-164.160,5.068-101.360,14.008-280.160,12.392-247.840 and 1.029-20.576μg·ml-1(r=0.9995-0.9998),respectively.The average recovery was 94.9%,95.9%,96.9%,101.6%,97.3%,98.2%,99.3%,99.9%,97.0%and 94.8%with the corresponding RSD of 1.1%,1.1%,0.2%,1.0%,0.7%,1.1%,0.4%,0.4%,0.5%and 1.2%(n=6),respectively.Conclusion:The method is available with high specificity,good reproducibility and high sensitive.It is suitable for the determination of 10 constituents in Xiaoshuan Tongluo tablets,which provides foundation for the perfect quality evaluation standard of Xiaoshuan Tongluo tablets.

关 键 词：消栓通络片 高效液相色谱-二极管阵列检测-蒸发光散射检测 毛蕊异黄酮葡萄糖苷 阿魏酸 芦丁 金丝桃苷 丹酚酸B 肉桂酸 三七皂苷R1 人参皂苷RG1 人参皂苷RB1 黄芪甲苷 

分 类 号：R927.2[医药卫生—药学]