HPLC法同时测定六味能消丸中8种成分的含量
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篇名: HPLC法同时测定六味能消丸中8种成分的含量
TITLE:
摘要: 目的:建立同时测定六味能消丸中土木香内酯、异土木香内酯、没食子酸、大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚含量的方法。方法:采用高效液相色谱法。色谱柱为Diamonsil C18,流动相为甲醇-乙腈-0.1%冰醋酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为254 nm(土木香内酯、异土木香内酯、大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚)、270 nm(没食子酸),柱温为25 ℃,进样量为10 μL。结果:土木香内酯、异土木香内酯、没食子酸、芦荟大黄素、大黄酸、大黄素、大黄素甲醚、大黄酚检测进样量线性范围分别为0.121~3.63 μg(r=0.999 9)、0.122~3.66 μg(r=0.999 9)、0.219~6.57 μg(r=0.999 9)、0.016 4~0.492 μg(r=0.999 7)、0.017 3~0.519 μg(r=0.999 9)、0.015 3~0.459 μg(r=0.999 9)、0.007 2~0.216 μg(r=0.999 9)、0.016 2~0.486 μg(r=0.999 9);定量限分别为0.41、0.26、0.35、0.13、0.17、0.14、0.15、0.13 ng,检测限分别为0.12、0.08、0.11、0.04、0.05、0.04、0.05、0.04 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为98.05%~102.46%(RSD=1.75%,n=6)、98.55%~102.89%(RSD=1.91%,n=6)、98.53%~102.34%(RSD=1.66%,n=6)、101.71%~103.41%(RSD=0.57%,n=6)、101.04%~103.01%(RSD=0.69%,n=6)、101.63%~102.75%(RSD=0.39%,n=6)、96.94%~101.11%(RSD=1.61%,n=6)、98.06%~99.10%(RSD=0.40%,n=6)。结论:该方法准确、简便,可用于六味能消丸中8种成分含量的同时测定。
ABSTRACT: OBJECTIVE: To establish the method for simultaneous determination of alantolactone, isoalantolactone, gallic acid, emodin, aloe-emodine, rhein, physcion and chrysophanol in Liuwei nengxiao pills. METHODS: HPLC method was adopted. The determination was performed on Diamonsil C18 with mobile phase consisted of methanol-acetonitrile-0.1% glacial acetic acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 254 nm (alantolactone, isoalantolactone, emodin, aloe-emodine, rhein, physcion and chrysophanol), 270 nm (gallic acid). The column temperature was 25 ℃, and sample size was 10 μL. RESULTS: The linear ranges of alantolactone, isoalantolactone, gallic acid, emodin,aloe-emodine, rhein, physcion,chrysosphanol were 0.121-3.63 μg(r=0.999 9),0.122-3.66 μg(r=0.999 9),0.219-6.57 μg(r=0.999 9), 0.016 4-0.492 μg(r=0.999 7),0.017 3-0.519 μg(r=0.999 9),0.015 3-0.459 μg(r=0.999 9),0.007 2-0.216 μg(r=0.999 9),0.016 2-0.486(r=0.999 9). The limits of quantification were 0.41, 0.26, 0.35, 0.13, 0.17, 0.14, 0.15, 0.13 ng; limits of detection were 0.12, 0.08, 0.11, 0.04, 0.05, 0.04, 0.05, 0.04 ng. RSDs of precision, stability and reproducibility tests were all lower than 2.0%. The recoveries were 98.05%-102.46%(RSD=1.75%,n=6),98.55%-102.89%(RSD=1.91%,n=6),98.53%-102.34%(RSD=1.66%,n=6),101.71%-103.41%(RSD=0.57%,n=6),101.04%-103.01%(RSD=0.69%,n=6),101.63%-102.75%(RSD=0.39%,n=6),96.94%-101.11%(RSD=1.61%,n=6),98.06%-99.10%(RSD=0.40%,n=6).  CONCLUSIONS: The method is accurate, simple and suitable for simultaneous determination of 8 components in Liuwei nengxiao pills.
期刊: 2017年第28卷第24期
作者: 康慧,刘亚蓉
AUTHORS: KANG Hui,LIU Yarong
关键字: 六味能消丸;土木香内酯;异土木香内酯;没食子酸;大黄素;芦荟大黄素;大黄酸;大黄素甲醚;大黄酚;高效液相色谱法;含量
KEYWORDS: Liuwei nengxiao pill; Alantolactone; Isoalantolactone; Gallic acid; Emodin; Aloe-emodine; Rhein; Physcion; Chrysophanol; HPLC; Content
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