HPLC-PDA法同时测定大黄蛰虫丸中6种成分的含量
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篇名: HPLC-PDA法同时测定大黄蛰虫丸中6种成分的含量
TITLE:
摘要: 目的:建立同时测定大黄蛰虫丸中苦杏仁苷、芍药苷、黄芩苷、甘草酸、大黄素及大黄酚含量的方法。方法:采用高效液相色谱法。色谱柱为Welchrom-C18,流动相为甲醇-0.1%磷酸(梯度洗脱),流速为1.0 mL/min,柱温为30 ℃,检测波长为210 nm(苦杏仁苷)、230 nm(芍药苷、黄芩苷)和250 nm[甘草酸(以甘草酸铵计)、大黄素、大黄酚],进样量为10 μL。结果:苦杏仁苷、芍药苷、黄芩苷、甘草酸、大黄素及大黄酚检测质量浓度线性范围分别为21.028~157.71、12.052~90.390、34.288~257.16、8.252 0~61.890、3.272 0~24.540、4.768 0~35.760 μg/mL(r均≥0.999 2);检测限分别为0.105 0、0.121 0、0.068 6、0.082 5、0.024 6、0.0179    μg/mL;定量限分别为0.263 0、0.362 0、0.171 0、0.268 0、0.065 5、0.047 7 μg/mL;精密度、稳定性(12 h)、重复性试验的RSD均<2.00%(n=6);加样回收率分别为96.01%~100.76%、97.09%~101.86%、99.70%~101.99%、96.29%~99.52%、98.47%~102.14%、97.19%~99.16%,RSD分别为1.63%、1.50%、0.82%、1.35%、1.35%、0.69%(n=6)。结论:该方法准确、简便、重复性好,可用于同时测定大黄蛰虫丸中苦杏仁苷、芍药苷、黄芩苷、甘草酸、大黄素及大黄酚的含量。
ABSTRACT: OBJECTIVE: To establish a method for amygdalin, paeoniforin, baicalin, glycyrrhizic acid, emodin and chrysophanol in Dahuang zhechong pills. METHODS: HPLC method was adopted. The determination was performed on Welchrom C18 with mobile phase consisted of methanol-0.1% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃, and the detection wavelengths were set at 210 nm (amygdalin), 230 nm (paeoniforin, baicalin) and 250 nm [glycyrrhizic acid (calculated with ammonium glycyrrhizinate), emodin, chrysophanol]. The sample size was 10 μL. RESULTS: The linear ranges of amygdalin,paeonifiorin,baicalin,ammonium glycyrrhizinate, emodin and chrysophanol fell within the ranges of 21.028-157.71,2.052-90.390, 34.288-257.16, 8.252 0-61.890, 3.272 0-24.540,4.768 0-35.760 μg/mL (all r≥0.999 2). The limits of detection were 0.105 0, 0.121 0, 0.068 6, 0.082 5, 0.024 6, 0.017 9 μg/mL. The limits of quantitation were     0.263 0, 0.362 0, 0.171 0, 0.268 0, 0.065 5, 0.047 7 μg/mL. RSDs of precision, stability(12 h)and reproducibility tests were lower than 2.00% (n=6). The  average  recoveries were 96.01%-100.76% (RSD=1.63%,n=6), 97.09%-101.86% (RSD=1.50%,n=6), 99.70%-101.99%(RSD=0.82%,n=6),96.29%-99.52%(RSD=1.35%,n=6), 98.47%-102.14% (RSD=1.35%, n=6) and 97.19%-99.16%(RSD=0.69%,n=6),respectively. CONCLUSIONS: The method is accurate, simple and reproducible for simultaneous determination of amygdalin, paeoniforin, baicalin, glycyrrhizic acid, emodin and chrysophanol in Dahuang zhechong pills.
期刊: 2019年第30卷第1期
作者: 张桂平,王东旭
AUTHORS: ZHANG Guiping,WANG Dongxu
关键字: 大黄蛰虫丸;苦杏仁苷;芍药苷;黄芩苷;甘草酸铵;大黄素;大黄酚;高效液相色谱法;含量测定
KEYWORDS: Dahuang zhechong pills; Amygdalin;Paeonifiorin;Baicalin;Glycyrrhizic acid;Emodin;Chrysophanol;HPLC; Content determination
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