HPLC法同时测定大黄-黄连药材中5种蒽醌类成分的含量及最优配伍研究
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篇名: HPLC法同时测定大黄-黄连药材中5种蒽醌类成分的含量及最优配伍研究
TITLE:
摘要: 目的:建立同时测定大黄-黄连药材中5种蒽醌类成分含量的方法,并优选大黄-黄连药材质量比。方法:采用高效液相色谱法。色谱柱为Zorbax SB-C18(250 mm× 4.6 mm,5 μm),流动相为乙腈-0.05 mol/L 磷酸二氢钾(48 ∶ 52,V/V,每100 mL中加十二烷基硫酸钠0.4 g,磷酸调节pH 至4.0),流速为1 mL/min,检测波长为254 nm,柱温为25 ℃,进样量为10 μL。考察大黄-黄连药材质量比为1 ∶ 1、1 ∶ 2、2 ∶ 1、2 ∶ 3、3 ∶ 2时配伍药材中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量。结果:芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚进样量分别在0.652~3.081、0.704~3.422、1.280~6.197、0.633~0.324、1.326~5.954 μg范围内与各自峰面积积分值呈良好线性关系(r≥0.999 7),精密度、稳定性、重复性试验的RSD均小于2.0%(n=6),平均加样回收率为98.92%~100.37%(RSD≤2.26%,n=6)。大黄-黄连药材质量比为2 ∶ 1时,5种蒽醌类成分总量最高。结论:本方法精密度、稳定性、重复性良好,可用于不同配伍比大黄-黄连药材的质量检定;大黄-黄连药材的最佳质量比为2 ∶ 1。
ABSTRACT: OBJECTIVE: To establish a method for the simultaneous content determination 5 anthraquinones of rhei radix-coptidis rhizoma, and optimize its best mass ratio. METHODS: HPLC was performed on the column of Zorbax SB-C18 (250 mm×4.6 mm, 5 μm) with mobile phase of acetonitrile-0.05 mol/L potassium dihydrogen phosphate (48 ∶ 52,   V/V, adding sodium dodecyl sulfate 0.4 g per 100 mL, pH value was adjusted to 4.0); detection wavelength was 254 nm; flow rate was 1 mL/min; column temperature was 25 ℃; and injection volume was 10 μL. When mass ratio of rhei radix-coptidis rhizoma was 1 ∶ 1, 1 ∶ 2, 2 ∶ 1, 2 ∶ 3, 3 ∶ 2, the contents of aloe emodin, rhein, emodin, chrysophanol and emodin ether were investigated. RESULTS: The aloe emodin, rhein, emodin, chrysophanol and emodin ether showed good linear relationship with peak area in the range of 0.652-3.081, 0.704-3.422, 1.280-6.197, 0.633-0.324, 1.326-5.954 μg (r≥0.999 7); RSDs of precision, stability, reproducibility tests were lower than 2.0% (n=6); and average recovery was 98.92%-100.37% (RSD≤2.26%, n=6). When mass ratio was 2 ∶ 1, the total contents of 5 ingredients were the highest. CONCLUSIONS: The method has good precision, stability, reproducibility, and can be used for the quality verification of rhei radix-coptidis rhizoma under different compatibilities. The best mass ratio of rhei radix-coptidis rhizoma is 2 ∶ 1.
期刊: 2017年第28卷第34期
作者: 王有森,王智亮
AUTHORS: WANG Yousen,WANG Zhiliang
关键字: 大黄;黄连;配伍;蒽醌类成分;高效液相色谱法
KEYWORDS: Rhei radix; Coptidis rhizoma; Compatibility; Anthraquinones; HPLC
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