HPLC法同时测定不同配伍比例黄连-吴茱萸药对中4种有效成分的含量
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篇名: HPLC法同时测定不同配伍比例黄连-吴茱萸药对中4种有效成分的含量
TITLE:
摘要: 目的:建立同时测定黄连-吴茱萸药对中4种有效成分含量的方法,探讨该药对的合理比例。方法:采用高效液相色谱法。色谱柱为Welch XB C18,流动相为乙睛-1.5 mmol/L十二烷基硫酸钠溶液(磷酸调pH至5.0 )(梯度洗脱),流速为1.0 mL/min,检测波长为265 nm,柱温为30 ℃,进样量为10 μL。结果:盐酸小檗碱、盐酸巴马汀、吴茱萸碱、吴茱萸次碱检测质量浓度线性范围分别为2.24~44.80 μg/mL(r=0.999 9)、1.26~31.50 μg/mL(r=0.999 8)、2.70~81.00 μg/mL(r=0.999 8)、1.65~49.50 μg/mL(r=0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为98.11%~100.73%(RSD=1.04%,n=6)、96.54%~103.47%(RSD=1.86%,n=6)、95.49%~102.36%(RSD=2.05%,n=6)、97.19%~103.24%(RSD=2.19%,n=6)。当黄连-吴茱萸比例(m/m)为2 ∶ 1时,各成分综合含量最高。结论:该方法操作简便,精密度、稳定性、重复性好,可用于不同配伍比例黄连-吴茱萸药对中4种有效成分含量的同时测定;该药对中黄连-吴茱萸比例(m/m)为2 ∶ 1较合理。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of 4 effective components in the couple of Coptidis Rhizoma and Evodiae Fructus,and to investigate rational proportion of the couple. METHODS: HPLC method was adopted. The determination was performed on Welch XB C18 column with mobile phase consisted of acetonitrile-1.5 mmol/L sodium dodecyl sulfate solution (pH adjusted to 5.0 with phosphoric acid) (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 265 nm, and the column temperature was 30 ℃. The sample size was 10 μL. RESULTS: The linear ranges of berberine hydrochloride, martin hydrochloride, evodiamine and rutacarpine were 2.24-44.80 μg/mL(r=0.999 9), 1.26-31.50 μg/mL(r=0.999 8), 2.70-81.00 μg/mL(r=0.999 8), 1.65-49.50 μg mL(r=0.999 9), respectively. RSDs of precision, stability and reproducibility tests were all lower than 3.0%. The recoveries were 98.11%-100.73%(RSD=1.04%,n=6),96.54%-103.47%(RSD=1.86%,n=6), 95.49%-102.36%(RSD=2.05%,n=6), 97.19%-103.24%(RSD=2.19%,n=6), respectively. When the proportion of Coptidis Rhizoma-Evodiae Fructus(m/m) was 2 ∶ 1, the comprehensive content of each component was the highest. CONCLUSIONS: The method is simple, accurate, stable and reproducible, and can be used for simultaneous determination of 4 effective components in different compatibility proportions of the couple of Coptidis Rhizoma and Evodiae Fructus. The rational proportion of the couple of Coptidis Rhizoma and Evodiae Fructus is 2 ∶ 1.
期刊: 2017年第28卷第24期
作者: 周素芹,李洪兵
AUTHORS: ZHOU Suqin,LI Hongbing
关键字: 黄连;吴茱萸;药对;高效液相色谱法;盐酸小檗碱;盐酸巴马汀;吴茱萸碱;吴茱萸次碱;含量测定
KEYWORDS: Coptidis Rhizoma;Evodiae Fructus;Couple; HPLC; Berberine hydrochloride; Martin hydrochloride; Evodia alkaloid; Rutacarpine; Content determination
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