RP-HPLC同时测定三黄片中4种有效成分的含量

 目的利用梯度洗脱,建立了反相高效液相色谱法同时测定三黄片中大黄素、大黄酚、黄芩苷和盐酸小檗碱含量的方法。方法采用Kromasil C₁₈色谱柱(4.6 mm×250 mm,5.0μm);流动相组成为A:0.5%三乙胺水溶液(醋酸调pH 3.0,内含5mmol·L^-1十二烷基磺酸钠),B:甲醇,C:乙腈,梯度洗脱;检测波长254 nm;流速1.0 mL·min^-1。结果大黄素、大黄酚、黄芩苷和盐酸小檗碱含量测定方法的线性关系良好,线性范围和相关系数分别为0.26～32.88 mg·L^-1(r=0.999 9),0.54～68.88 mg·L^-1(r=0.999 9),9.83～1 258 mg·L^-1(r=0.999 7),3.07～392.8 mg·L^-1(r=0.999 8);回收率分别为99.7%,100.2%,100.2%和98.0%,方法精密度良好,RSD均小于2.0%,方法的重现性良好,RSD均小于1.3%。结论该方法专属性强,结果准确可靠,重现性好,可用于三黄片中大黄素、大黄酚、黄芩苷和盐酸小檗碱的含量测定,更好地控制三黄片的质量。

Simultaneous Determination of Rhein, Emodin, Baicalina and Berberine Hydrochloride in Sanhuang Tablets by RP-HPLC

OBJECTIVE To develop a quantitative RP-HPLC method for the determination of rhein,emodin,baicalina,berberine hydrochloride in Sanhuang tablets.METHODS A column of Kromasil C₁₈(4.6 mm×250 mm,5 μm) was used.The mobile phase composed of 0.5% triethylamine (pH 3.0,contented 5 mmol·L^-1SDS)(A),methanol(B) and acetonitrile(C) with gradient elution.The flow rate was 1.0 mL·min^-1 with UV detection wavelength at 254 nm.RESULTS A good linearity was obtained with the correlation coefficients ranged from 0.26～32.88 mg·L^-1(r=0.999 9),0.54～68.88 mg·L^-1(r=0.999 9),9.83～1 258 mg·L^-1(r=0.999 7),3.07～392.8 mg·L^-1((r=0.998 8)).The average recoveries were 99.7%,100.2%,100.2% and 98.0% with corresponding RSDs of 0.9%～1.8%,respectively.The precision and accuracy of the assay were not more than 1.3%(n=5).CONCLUSION The method is rapid,accurate,reliable and can be used to control the quality of Sanhuang tablets.