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作 者:杨洪早 王东升[1] 苗小楼[1] 张世栋[1] 董书伟[1] 闫宝琪 桑梦琪 那立冬 严作廷[1] YANG Hong-zao1,2, WANG Dong-sheng1, MIAO Xiao-lou1, ZHANG Shi-dong1, DONG Shu-wei1, YAN Bao-qi1, SANG Meng1, NA Li-dong1,2, YAN Zuo-ting1(1. Lanzhou Institute of Animal Husbandry and Pharmaceutical Sciences, Chinese Academy of Agricultural Sciences/ Key Laboratory of Veterinary Pharmaceutical Discovery, Ministry of Agricuiture , Lanzhou 730050, China 2. College of Veterinary Medicine, Gansu Agricultural University, Lanzhou 730070, Chin)
机构地区:[1]中国农业科学院兰州畜牧与兽药研究所/中国农业部兽用药物创制重点实验室,兰州730050 [2]甘肃农业大学动物医学院,兰州730070
出 处:《西南大学学报(自然科学版)》2018年第3期1-9,共9页Journal of Southwest University(Natural Science Edition)
基 金:中国农业科学院科技创新工程项目(CAAS-ASTIP-2014-LIHPS-03);"十二五"国家科技支撑计划重点课题(2012BAD12B03)
摘 要:目的建立藿芪灌注液质量标准.方法采用薄层色谱法对处方中淫羊藿、红花、丹参与益母草进行TLC定性鉴别;使用WondaSil C18柱(4.6mm×250mm,5μm),流动相∶乙腈-水(28∶72),柱温40℃,检测波长270nm,进样量10μL,流速1.0mL/min测定淫羊藿苷的含量;使用ZORBAX SB-C18柱(4.6mm×150mm,5μm),漂移管温度为90℃,载气流速为2.5L/min,流动相∶甲醇-水(65∶35),柱温40℃,流速1mL/min,用蒸发光散射检测器测定黄芪甲苷的含量.结果 TLC鉴别色谱图分离效果好,阴性对照无干扰,专属性强,重复性好;测定淫羊藿苷与黄芪甲苷含量表明,分别在2.336~58.4μg/mL(r=0.999 9)和0.047 8~0.478mg/mL(r=0.999 6)范围内与峰面积成较好的线性关系;其平均加样回收率分别为100.2%,RSD=0.45%和99.26%,RSD=1.46%.结论所建立的特征图谱专属性强、准确可行、简便、可快速用于定性鉴别、定量检测,可有效地用于该制剂的质量控制方法.Objective To establish the quality standard for Huoqi perfusion.Methods TLC was used for qualitative identification of Epimedium,Carthamus tinctorius,Salvia miltiorrhiza and Leonuri herba.The separation of icariin was achieved by a WondaSil-C18 column(4.6 mm×250 mm,5μm),with a mobile phase composed of acetonitrile-water(28∶72),a detection wavelength of 270 nm,a column temperature of 40 ℃.an injection volume of 10μL and a flow rate of 1.0 mL/min.The separation of the astragaloside was achieved by a ZORBAX SB-C18 column(4.6 mm×150 mm,5μm)with a drift tube temperature of 90 ℃,a carrier gas flow rate of 2.5 L/min and a mobile phase composed of methanol-water(65∶35).The flow rate was 1.0 mL/min and the column temperature was 40 ℃,with an evaporative light scattering detector.Results The spots on TLC plates were clear without interference by the blank reference and with good specificity and repeatability.The linear ranges of icariin and astragaloside were obtained between2.336-58.4μg/mL(r=0.999 97)and 0.047 8-0.478 mg/mL(r=0.999 6),the recovery averaging100.2%(RSD =0.45%)and 99.26%(RSD =1.46%),respectively.Conclusion The determination method reported in this paper is specific,accurate,feasible,simple and convenient,and can be used for the determination of the active ingredients of the preparation,which provides a reference value for the quality standard of the preparation.
关 键 词:藿芪灌注液 薄层色谱法 高效液相色谱法 红花 丹参 益母草 淫羊藿苷 黄芪甲苷
分 类 号:S853.7[农业科学—临床兽医学]
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