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复方鱼腥草胶囊中连翘苷和黄芩苷的高效液相色谱法含量检测 被引量:6

Detection of the Content of Forsythia and Baicalin in Fufang Yuxingcao Capsules by High Performance Liquid Chromatography
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摘要 目的:评价采用高效液相指纹图谱分析复方鱼腥草胶囊中连翘苷和黄芩苷的含量。方法:首先制备复方鱼腥草胶囊供试品溶液及连翘苷、黄芩苷对照品溶液,通过文献检索和预实验优化高效液相色谱法(HPLC)指纹图谱的条件,色谱条件为采用ACQUITY-BEHP-henyl-C_(18)保护柱(5μm),以室内温度为柱温,进样量为20μL以乙腈为流动相A,以水+0. 02%磷酸为流动相B,流速1. 0 mL/min:检测波长为327 nm;进行线性回归、精密度、重复性、稳定性、专属性试验和加样回收率试验,考察HPLC方法学的严谨性,检测样品中连翘苷和黄芩苷的含量。结果:复方鱼腥草胶囊中连翘和黄芩专属性良好。连翘苷回归方程Y=98 009X-86 650,r=0. 999 2(n=5),连翘苷对照品在3. 23~103. 02μg/mL范围内线性关系良好;黄芩苷回归方程Y=212 284 X+108 806,r=0. 999 8(n=5),黄芩苷对照品在2. 74~87. 89μg/mL范围内线性关系良好。薄层色谱法鉴别连翘苷和黄芩苷经365 nm的紫外灯观察发现连翘苷和黄芩苷在阴性对照品位置上相互之间不存在干扰现象。样品1连翘苷含量0.51 mg,RSD为1.72%,黄芩苷含量14. 6 mg,RSD为4. 95%;而样品2连翘苷0. 50mg,RSD为1. 69%,黄芩苷含量14.3 mg,RSD为4. 92%; 2组复方鱼腥草胶囊样品中连翘苷和黄芩苷的含量差异无统计学意义(P> 0. 05)。结论:复方鱼腥草胶样品质量可控性、稳定性和专属性均较好。 Objective:To analyze the content of forsythia and baicalin in Fufang Yuxingcao capsules by high performance liquid chromatography(HPLC)fingerprint.Methods:The Fufang Yuxingcao capsule test solution and phillyrin and baicalin control solution were prepared.Through literature search and pre experiment,HPLC fingerprint was optimized.The chromatographic conditions were ACQUITY-BEHP-henyl-C 18 protection column(5μm).Indoor temperature was column temperature.Injection volume was 20μL.Acetonitrile was mobile phase A,and water+0.02%phosphoric acid was mobile phase B.Flow rate was 1.0 mL/min:Detection wavelength was 327 nm.Linear regression,precision,repeatability,stability,specificity test and sample recovery test were performed to observe the rigor stringency of HPLC method.The contents of phillyrin and baicalin in the samples were detected.Results:1)HPLC chromatography was applied to the specific test of Fructus Forsythiae and Radix Scutellariae in Fufang Yuxingcao capsule,which had good specificity.2)Forsyth regression equation Y=98009X-86650,r=0.9992(n=5),and the linearity of phillyrin control in 3.23~103.02μg/mL was good;Baicalin regression equation Y=212284X+108806,r=0.9998(n=5),and the linearity of baicalin control in 2.74~87.89μg/mL was good.3)Identification of forsythin and baicalin by 365 nm showed that there was no interference between forsythin and baicalin in the location of negative controls.4)Samples 1∶0.51 mg of phillyrin,RSD 1.72%;14.6 mg of baicalin,RSD 4.95%.Sample 2:0.50 mg phillyrin,RSD 1.69%;14.3 mg baicalin,RSD 4.92%.There was no significantly difference between phillyrin and baicalin in Fufang Yuxingcao capsule samples(P>0.05).Conclusion:The quality control,stability and specificity of the Fufang Yuxingcao capsule sample are good.
作者 周宝玉 虞文妹 Zhou Baoyu;Yu Wenmei(TCM Pharmacy,Wujin Hospital of Traditional Chinese Medicine Affiliated to Nanjing University of Chinese Medicine,Nanjing 213161,China)
出处 《世界中医药》 CAS 2018年第12期3186-3189,共4页 World Chinese Medicine
基金 国家中医药管理局全国中药特色技术传承人才培训项目[国中医药人函(2015)168]
关键词 高效液相色谱 指纹图谱 复方鱼腥草胶囊 连翘苷 黄芩苷 含量检测 稳定性 专属性 High performance liquid phase Fingerprint Fufang Yuxingcao capsule Forsythia Baicalin Content detection Stability Specificity
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