HPLC法同时测定通窍耳聋丸中7个成分的含量  

Simultaneous determination of seven constituents in Tongqiao Erlong pills by HPLC

作　　者：胡小祥 陈新明 何艳 蒋建宏 周佳男 HU Xiao-xiang;CHEN Xin-ming;HE Yan;JIANG Jian-hong;ZHOU Jia-nan(Chenzhou Municipal Center for Food and Drug Control,Chenzhou 423000,China;College of Pharmacy,Xiangnan University,Chenzhou 423000,China;College of Chemical Biology and Environmental Engineering Xiangnan University,Chenzhou 423000,China)

机构地区：[1]郴州市食品药品检验检测中心,郴州423000 [2]湘南学院药学院,郴州423000 [3]湘南学院化学生物与环境工程学院,郴州423000

出　　处：《药物分析杂志》2021年第8期1381-1388,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：湖南省“双一流”药学应用特色学科基金(湘教通[2018]469号);湖南省大学生创新创业训练计划项目(项目编号:S202010545008)。

摘　　要：目的:建立高效液相色谱法同时测定通窍耳聋丸中龙胆苦苷、栀子苷、黄芩苷、汉黄芩苷、黄芩素、木香烃内酯、大黄酚的含量。方法:供试品以70%甲醇水回流提取1 h,采用Waters Atlantis T3-C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.15%磷酸水溶液,梯度洗脱,流速1.0 mL·min-1,柱温30℃,检测波长240 nm(检测龙胆苦苷和栀子苷)、278 nm(检测黄芩苷、汉黄芩苷和黄芩素)、224 nm(检测木香烃内酯和大黄酚),进样量10μL。对16批样品进行聚类分析。结果:龙胆苦苷、栀子苷、黄芩苷、汉黄芩苷、黄芩素、木香烃内酯、大黄酚的线性范围分别为3.256~32.56μg·mL^(-1)(r=0.9999)、5.303~53.03μg·mL^(-1)(r=0.9998)、23.74~273.4μg·mL^(-1)(r=0.9997)、5.721~57.21μg·mL^(-1)(r=0.9999)、2.174~21.74μg·mL^(-1)(r=0.9999)、2.283~22.83μg·mL^(-1)(r=0.9999)、1.053~10.53μg·mL^(-1)(r=0.9998);平均加样回收率(n=6)分别为100.9%、101.6%、101.1%、98.5%、100.7%、98.4%、98.8%,RSD分别为1.3%、1.3%、1.9%、2.0%、2.6%、1.4%、2.5%。16批样品中龙胆苦苷、栀子苷、黄芩苷、汉黄芩苷、黄芩素、木香烃内酯、大黄酚的含量分别为0.3900~2.038、1.912~3.560、10.40~14.34、2.118~3.745、0.1898~1.324、0.2914~0.7843、0.2300~0.5459 mg·g^(-1),16批样品可分为2类。结论:该方法准确,重复性和耐用性好,可用于通窍耳聋丸的质量控制和评价。Objective:To develop an HPLC method for simultaneous determination of gentiopicroside,geniposide,baicalin,wogonoside,baicalein,costunolide and chrysophanol in Tongqiao Erlong pills.Methods:The sample was extracted with 70%methanol by refluxing for 1h.The analysis was performed on a Waters Atlantis T3-C_(18) column(250 mm×4.6 mm,5μm)by gradient elution of acetonitrile-0.15%phosphoric acid solution at a flow rate of 1.0 mL·min-1.The column temperature was set at 30℃,the injection volume was 10μL,and the detection wavelengths were set at 240 nm(detecting gentiopicroside and geniposide),278 nm(detecting baicalin,wogonoside and baicalein)and 224 nm(detecting costunolide and chrysophanol).Cluster analysis was conducted in 16 batches of samples.Results:The linear ranges of gentiopicroside,geniposide,baicalin,wogonoside,baicalein,costunolide and chrysophanol were 3.256-32.56μg·mL^(-1)(r=0.9999),5.303-53.03μg·mL^(-1)(r=0.9998),23.74-273.4μg·mL^(-1)(r=0.9997),5.721-57.21μg·mL^(-1)(r=0.9999),2.174-21.74μg·mL^(-1)(r=0.9999),2.283-22.83μg·mL^(-1)(r=0.9999)and 1.053-10.53μg·mL^(-1)(r=0.9998),respectively.The average recoveries were 100.9%,101.6%,101.1%,98.5%,100.7%,98.4%and 98.8%,and the RSDs were 1.3%,1.3%,1.9%,2.0%,2.5%,1.4%and 2.5%,respectively.The contents of the seven components in 16 batches of samples were 0.3900-2.038,1.912-3.560,10.40-14.34,2.118-3.745,0.1898-1.324,0.2914-0.7843 and 0.2300-0.5459 mg·g^(-1),respectively.16 batches of samples were clustered into two categories.Conclusion:This accurate,reproducible and durable method can be used for quality control and quality evaluation of Tongqiao Erlong pills.

关 键 词：通窍耳聋丸 高效液相色谱 龙胆苦苷 栀子苷 黄芩苷 汉黄芩苷 黄芩素 木香烃内酯 大黄酚 含量测定 

分 类 号：R917[医药卫生—药物分析学]