HPLC法同时测定舒肝和胃丸中5种成分的含量
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篇名: HPLC法同时测定舒肝和胃丸中5种成分的含量
TITLE: Simultaneous Determination of 5 Components in Shugan Hewei Pills by HPLC
摘要: 目的:建立同时测定舒肝和胃丸中7-羟基香豆素、6,7-二甲氧基香豆素、5,7-二甲氧基香豆素、欧前胡素、佛手柑内酯等5种成分含量的方法。方法:采用索氏提取法对舒肝和胃丸进行提取,经D101型大孔吸附树脂分离后,采用高效液相色谱法测定上述5种成分的含量。色谱柱为VenusilMPC18,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270nm,柱温为30℃,进样量为10μL。结果:7-羟基香豆素、6,7-二甲氧基香豆素、5,7-二甲氧基香豆素、欧前胡素、佛手柑内酯检测质量浓度的线性范围分别为1.875~187.5μg/mL(r=0.9999)、1.075~107.5μg/mL(r=0.9999)、1.261~126.1μg/mL(r=0.9999)、0.875~87.5μg/mL(r=0.9999)、2.033~203.3μg/mL(r=0.9998),精密度、稳定性(24h)、重复性、耐用性试验的RSD均小于2.0%,平均加样回收率分别为95.18%~98.44%(RSD=1.27%,n=6)、95.35%~98.14%(RSD=1.16%,n=6)、95.21%~97.32%(RSD=0.83%,n=6)、95.43%~97.14%(RSD=0.76%,n=6)、95.12%~98.75%(RSD=1.35%,n=6)。3批舒肝和胃丸中上述5种成分的平均含量分别为0.424、0.239、0.305、0.180、0.459mg/g(n=2)。结论:成功建立了可同时测定舒肝和胃丸中5种成分含量的方法。
ABSTRACT: OBJECTIVE:To establish a method for sim ultaneous determination of 7-hydroxycoumarin,6,7-dimethoxy- coumarin,5,7-dimethoxycoumarin,imperatorin and bergaptene in Shugan hewei pills. METHODS :Samples were extracted by Soxhlet extraction and separated by using D 101 macroporous adsorption resin ;HPLC method was used to determine the contents of above 5 components. The determination was performed on Venusil MP C 18 column with mobile phase consisted of methanol- 0.1% phosphoric acid water solution (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelength was 270 nm and the column temperature was 30 ℃ . The sample size was 10 μ L. RESULTS:The linear ranges were 1.875-187.5 μ g/mL for 7-hydroxycoumarin(r=0.999 9),1.075-107.5 μg/mL for 6,7-dimethoxycoumarin(r=0.999 9),1.261-126.1 μg/mL for 5, 7-dimethoxycoumarin(r=0.999 9),0.875-87.5 μg/mL for imperatorin(r=0.999 9),2.033-203.3 μg/mL for bergaptene(r=0.999 8), respectively. RSDs of precision ,stability(24 h),reproducibility and durability tests were lower than 2.0%. Average recoveries were 95.18% -98.44% (RSD=1.27% ,n=6), 95.35% -98.14% (RSD=1.16% ,n=6),95.21% -97.32% (RSD=0.83% ,n=6), 95.43%-97.14%(RSD=0.76%,n=6),95.12%-98.75%(RSD=1.35%,n=6),respectively. The average contents of the above five components in 3 batches of shugan hewei pills were 0.424,0.239,0.305,0.180,0.459 mg/g(n=2).CONCLUSIONS:A method for simultaneous determination of five components in Shugan hewei pills was established.
期刊: 2020年第31卷第14期
作者: 宫兴华,郑磊,李娟
AUTHORS: GONG Xinghua ,ZHENG Lei,LI Juan
关键字: 舒肝和胃丸;高效液相色谱法;含量测定;7-羟基香豆素;6,7-二甲氧基香豆素;5,7-二甲氧基香豆素;欧前胡素;佛手柑
KEYWORDS: Shugan hewei pills ; HPLC; Content determination ; 7-hydroxycoumarin; 6,7-dimethoxycoumarin; 5,
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