HPLC法同时测定桂枝加芍药汤中8种成分的含量
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篇名: | HPLC法同时测定桂枝加芍药汤中8种成分的含量 |
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摘要: | 目的:建立同时测定桂枝加芍药汤中芍药内酯苷、芍药苷、甘草苷、甘草素、肉桂酸、桂皮醛、甘草酸铵、6-姜酚含量的方法。方法:采用高效液相色谱法。色谱柱为Kromasil C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为235 nm(0~35 min,芍药内酯苷、芍药苷、甘草苷)、280 nm(35~65 min,甘草素、肉桂酸、桂皮醛、甘草酸铵、6-姜酚),柱温为25 ℃,进样量为20 μL。结果:芍药内酯苷、芍药苷、甘草苷、甘草素、肉桂酸、桂皮醛、甘草酸铵、6-姜酚检测质量浓度线性范围分别为2.125~34.000 μg/mL(r=0.999 9)、28.700~459.200 μg/mL(r=0.999 7)、3.675~58.800 μg/mL(r=0.999 7)、1.235~19.760 μg/mL(r=0.999 8)、2.300~36.800 μg/mL(r=0.999 8)、0.955~15.280 μg/mL(r=0.999 7)、36.000~576.000 μg/mL(r=0.999 7)、1.500~24.000 μg/mL(r=0.999 7);定量限分别为0.135、0.102、0.096、0.033、0.013、0.023、0.663、0.198 μg/mL,检测限分别为0.041、0.031、0.029、0.010、0.004、0.007、0.201、0.059 μg/mL;精密度、稳定性、重复性试验的RSD均小于3%(n=6);加样回收率分别为97.47%~100.76%(RSD=1.33%,n=6)、98.15%~103.50%(RSD=1.82%,n=6)、95.65%~100.84%(RSD=2.38%,n=6)、96.75%~100.32%(RSD=1.31%,n=6)、95.88%~102.75%(RSD=2.52%,n=6)、95.63%~100.63%(RSD=2.00%,n=6)、96.78%~100.45%(RSD=1.35%,n=6)、95.71%~100.48%(RSD=1.80%,n=6)。结论:该方法准确、可靠,专属性好,可用于同时测定桂枝加芍药汤中8种成分的含量。 |
ABSTRACT: | OBJECTIVE: To establish a method for simultaneous determination of albiflorin, paeoniflorin, liquiritin, liquiritigenin, cinnamic acid, cinnamaldehyde, ammonium glycyrrhetate and 6-ginger phenol in Guizhijiashaoyao decoction. METHODS: HPLC method was adopted. The determination was performed on Kromasil C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were 235 nm(0-35 min,albiflorin, paeoniflorin, liquiritin)、280 nm(35-65 min,liquiritigenin, cinnamic acid, cinnamaldehyde, ammonium glycyrrhetate and 6-ginger phenol). The column temperature was 25 ℃, and the sample size was 20 μL. RESULTS: The linear range of albiflorin, paeoniflorin, liquiritin, liquiritigenin, cinnamic acid, cinnamaldehyde, ammonium glycyrrhetate and 6-ginger phenol were 2.125-34.000 μg/mL(r=0.999 9), 28.700-459.200 μg/mL(r=0.999 7), 3.675-58.800 μg/mL(r=0.999 7), 1.235-19.760 μg/mL(r=0.999 8), 2.300-36.800 μg/mL(r=0.999 8), 0.955-15.280 μg/mL(r=0.999 7), 36.000-576.000 μg/mL(r=0.999 7) and 1.500-24.000 μg/mL(r=0.999 7), respectively. The quantitative limits were 0.135, 0.102, 0.096, 0.033, 0.013, 0.023, 0.663, 0.198 μg/mL; the detection limits were 0.041, 0.031, 0.029, 0.010, 0.004, 0.007, 0.201, 0.059 μg/mL. RSDs of precision, stability and reproducibility tests were all lower than 3% (n=6). The recovery rates were 97.47%-100.76%(RSD=1.33%,n=6), 98.15%-103.50%(RSD=1.82%,n=6), 95.65%-100.84%(RSD=2.38%,n=6), 96.75%-100.32%(RSD=1.31%,n=6), 95.88%-102.75%(RSD=2.52%,n=6), 95.63%-100.63%(RSD=2.00%,n=6), 96.78%-100.45%(RSD=1.35%,n=6), 95.71%-100.48%(RSD=1.80%,n=6). CONCLUSIONS: The method is accurate, reliable and exclusive, and suitable for simultaneous determination of 8 ingredients in Guizhijiashaoyao decoction. |
期刊: | 2019年第30卷第6期 |
作者: | 韩真真,邵长森,张元元,王绍花,刘莉,林桂涛,盛华刚 |
AUTHORS: | HAN Zhenzhen,SHAO Changsen,ZHANG Yuanyuan,WANG Shaohua,LIU Li, LIN Guitao,SHENG Huagang |
关键字: | 桂枝加芍药汤;高效液相色谱法;含量测定;芍药内酯苷;芍药苷;甘草苷;甘草素;肉桂酸;桂皮醛;甘草酸铵;6-姜酚 |
KEYWORDS: | Guizhijiashaoyao decoction; HPLC; Content determination; Albiflorin; Paeoniflorin; Liquiritin; Liquiritigenin; Cinnamic acid; Cinnamaldehyde; Ammonium glycyrrhetate; 6-ginger phenol |
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