HPLC法测定圣愈汤冻干粉中4个指标成分的含量
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篇名: HPLC法测定圣愈汤冻干粉中4个指标成分的含量
TITLE: Content Determination of 4 Indicator Components in Shengyu Decoction Lyophilized Powder by HPLC
摘要: 目的:建立测定圣愈汤冻干粉中阿魏酸、毛蕊花糖苷、藁本内酯、黄芪甲苷含量的方法。方法:采用高效液相色谱法测定3批冻干粉样品4种成分含量。测定阿魏酸、毛蕊花糖苷、藁本内酯的色谱柱为InertsilODS-SPC18,流动相为甲醇-0.1%磷酸水溶液,梯度洗脱,流速为1.0mL/min,检测波长为330nm,检测器为二极管阵列检测器,柱温为30℃,进样量为10μL;测定黄芪甲苷的色谱柱为KromasilC18,流动相为乙腈-水(32∶68,V/V),检测器为蒸发光散射检测器,漂移管温度为100℃,载气(空气)流量为2.5L/min,流速为1.0mL/min,柱温为30℃,进样量为10μL。结果:阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷进样量线性范围分别为0.05015~10.03μg(r=0.9998)、0.06780~13.56μg(r=0.9999)、0.05730~11.46μg(r=0.9995)、1.128~11.28μg(r=0.9993);检测限分别为2.12×10-4、1.30×10-3、8.02×10-4、1.09×10-3μg,定量限分别为7.43×10-4、3.87×10-3、2.34×10-3、3.36×10-3μg;精密度、稳定性(12h)、重复性试验的RSD均小于2%(n=6);平均加样回收率分别为99.6%(RSD=0.83%,n=6)、100.9%(RSD=1.07%,n=6)、98.8%(RSD=0.84%,n=6)和101.3%(RSD=0.99%,n=6)。3批样品中阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷的含量分别为1.225~1.248、0.413~0.424、0.325~0.332、0.394~0.404mg/g(批间RSD<1.5%)。结论:建立的含量测定方法稳定性、重复性好,能够快速、准确地测定圣愈汤冻干粉中阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷的含量。
ABSTRACT: OBJECTIVE:To establish the content determin ation method of ferulic acid ,verbascoside,ligustilide and astragaloside in Shengyu decoction lyophilized powder. METHODS :HPLC method was adopted to determine 4 components in 3 batches of lyophilized powder. The determination of ferulic acid ,verbascoside and ligustilide was performed on Inertsil ODS-SP C 18 column with mobile phase consisted of methanol- 0.1% phosphoric acid (gradient elution )at the flow rate of 1.0 mL/min;detector was diode array detector ;detection wavelength was set at 330 nm;column temperature was 30 ℃,the sample size was 10 μL. The determination of astragaloside was performed on Kromasil C 18 column with mobile phase consisted of acetonitrile-water (32∶68,V/ V);detector was evaporative light scattering detector ;the drift tube temperature wa s 100 ℃,the carrier gas (air)flow rate was 2.5 L/min at the flow rate of 1.0 mL/min;column temperature was 30 ℃,the sample size was 10 μL. RESULTS:The linear ranges of ferulic acid ,verbascoside,ligustilide and astragaloside were 0.050 15-10.03 μg(r=0.999 8),0.067 80-13.56 μg(r= 0.999 9),0.057 30-11.46 μg(r=0.999 5),1.128-11.28 μg(r=0.999 3),respectively. The detection limits were 2.12×10-4,1.30× 10-3,8.02×10-4,1.09×10-3 μg,respectively. The limit of quantification were 7.43×10-4,3.87×10-3,2.34×10-3,3.36×10-3 μg, respectively. RSDs of precision ,stability(12 h)and reproducibility tests were all lower than 2%(n=6). Average recovery rates were 99.6%(RSD=0.83%,n=6),100.9%(RSD=1.07%,n=6),98.8%(RSD=0.84%,n=6)and 101.3%(RSD=0.99%, n=6),respectively. The contents of ferulic acid ,verbascoside,ligustilide and astragaloside in 3 batches of samples were 1.225-1.248, 0.413-0.424, 0.325-0.332, 0.394-0.404 mg/g, respectively (RSDs among batches were lower than 1.5% ). CONCLUSIONS:Established method is stable ,reproducible,rapid and accurate for the content determination of ferulic acid , verbascoside, ligustilide and astragaloside in Shengyu
期刊: 2020年第31卷第05期
作者: 董丹华,刘玉军,李亚男,胡祥昊,孙平,李婷,刘菊妍,高鹏
AUTHORS: DONG Danhua ,LIU Yujun,LI Yanan ,HU Xianghao ,SUN Ping,LI Ting,LIU Juyan,GAO Peng
关键字: 圣愈汤;冻干粉;高效液相色谱法;阿魏酸;毛蕊花糖苷;藁本内酯;黄芪甲苷;含量测定
KEYWORDS: Shengyu decoction ; Lyophilized powder ;
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