HPLC法同时测定青娥丸中7种成分的含量
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篇名: HPLC法同时测定青娥丸中7种成分的含量
TITLE:
摘要: 目的:建立同时测定青娥丸中补骨脂素、异补骨脂素、佛手柑内酯、欧前胡素、三甲基补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮含量的方法。方法:采用高效液相色谱法。色谱柱为Kinetex-C18,流动相为甲醇-0.1%乙酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为248 nm,柱温为30 ℃,进样量为20 μL。结果:补骨脂素、异补骨脂素、佛手柑内酯、欧前胡素、三甲基补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮检测质量浓度线性范围分别为1.012~101.2 μg/mL(r=0.999 9)、1.007~100.7 μg/mL(r=0.999 7)、1.010~101.0 μg/mL(r=0.999 9)、1.021~102.1 μg/mL(r=0.999 9)、1.002~100.2 μg/mL(r=0.999 6)、1.008~100.8 μg/mL(r=0.999 9)、1.025~102.5 μg/mL(r=0.999 8);定量限分别为0.15、0.15、0.30、0.30、0.15、0.30、0.30 μg/mL,检测限分别为0.05、0.05、0.10、0.10、0.05、0.10、0.10 μg/mL;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为95.3%~99.6%(RSD=1.9%,n=6)、96.1%~99.3%(RSD=1.2%,n=6)、95.2%~98.4%(RSD=1.4%,n=6)、95.4%~99.2%(RSD=1.5%,n=6)、96.1%~99.3%(RSD=1.5%,n=6)、95.6%~98.9%(RSD=1.4%,n=6)、95.2%~99.6%(RSD=1.6%,n=6)。结论:该方法简便、结果准确,适用于青娥丸中7种成分含量的同时测定。
ABSTRACT: OBJECTIVE: To develop a method for simultaneous determination of psoralen, isopsoralen, bergapten, imperatorin, trimethylpsorale, neobavaisoflavone and bavachin in Qing’e pills. METHODS: HPLC method was adopted. The separation was performed on Kinetex-C18 column with mobile phase consisted of methanol-0.1% glacial acetic (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 248 nm. The column temperature was 30 ℃. The sample size was 20 μL. RESULTS: The linear ranges were 1.012-101.2 μg/mL for psoralen (r=0.999 9),1.007-100.7 μg/mL for isopsoralen (r=0.999 7), 1.010-101.0 μg/mL for bergapten (r=0.999 9), 1.021-102.1 μg/mL for imperatorin (r=0.999 9), 1.002-100.2 μg/mL for trimethylpsorale (r=0.999 6), 1.008-100.8 μg/mL for neobavaisoflavone (r=0.999 9), 1.025-102.5 μg/mL for bavachin (r=0.999 8),respectively. The limits of quantitation were 0.15, 0.15, 0.30, 0.30, 0.15, 0.30, 0.30 μg/mL, and the limits of detection were 0.05, 0.05, 0.10, 0.10, 0.05, 0.10, 0.10 μg/mL,respectively. RSDs of precision, stability and reproducibility tests were lower than 2.0%. The recoveries were 95.3%-99.6% (RSD=1.9%,n=6), 96.1%-99.3% (RSD=1.2%,n=6), 95.2%-98.4% (RSD=1.4%,n=6), 95.4%-99.2%(RSD=1.5%,n=6), 96.1%-99.3%(RSD=1.5%,n=6), 95.6%-98.9% (RSD=1.4%,n=6), 95.2%-99.6% (RSD=1.6%,n=6), respectively. CONCLUSIONS: The method is simple and accurate, can be used for simultaneous determination of 7 kinds of components in Qing’e pills.
期刊: 2017年第28卷第33期
作者: 王向锋,黄小为,刘明霞,朱玉青
AUTHORS: WANG Xiangfeng,HUANG Xiaowei,LIU Mingxia,ZHU Yuqing
关键字: 高效液相色谱法;青娥丸;含量;补骨脂素;异补骨脂素;佛手柑内酯;欧前胡素;三甲基补骨脂素;新补骨脂异黄酮;补骨脂二氢黄酮
KEYWORDS: HPLC; Qing’e pills; Content; Psoralen; Isopsoralen; Bergapten; Imperatorin; Trimethylpsorale; Neobavaisoflavone; Bavachin
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