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纸质出版日期:2020,
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董丹华, 刘玉军, 李亚男, 等. HPLC法测定圣愈汤冻干粉中4个指标成分的含量[J]. 中国药房, 2020,31(5).
DONG Danhua, LIU Yujun, LI Yanan, et al. Content Determination of 4 Indicator Components in Shengyu Decoction Lyophilized Powder by HPLC[J]. China Pharmacy, 2020,31(5).
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。
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
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
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