藏药智托洁白丸中没食子酸的定性与定量检测

目的:建立智托洁白丸处方中没食子酸定性与定量测定方法。方法:定性测定采用薄层色谱法。定量测定采用高效液相色谱法,色谱柱为Sunfire-ODSC18柱(250mm,4.6mm),柱温30℃,以乙腈-含体积分数0.1%三乙胺的体积分数0.1%磷酸溶液(体积比3:97)为流动相;检测波长为273nm,理论板数按没食子酸峰计算不低于3000。结果:薄层色谱图中,供试品、对照药材和对照品在相应位置上显相同颜色的斑点,阴性对照无干扰。定量检测时,没食子酸进样量在0.0157～0.2830μg范围内线性关系良好,标准曲线为Y=4×107X+6532(R2=0.9998);方法的精密度和重现性均良好(RSD分别为0.05%,1.43%),12h内的稳定性良好(RSD=0.65%);平均回收率为98.07%,RSD=0.76%。9批样品中没食子酸平均含量为8.8mg/g。结论:所建立的薄层色谱定性检测方法和高效液相色谱定量检测方法可用于智托洁白丸中没食子酸的定性鉴别和定量控制。

Qualitative and quantitative determination of gallic acid in tibetan Zhi Tuo Jie Bai Wan

Aim:To establish the qualitative and quantitative determination methods of gallic acid in Zhi Tuo Jie Bai Wan.Methods:Thin layer chromatography(TLC) and high performance liquid chromatography(HPLC) were established for the qualitative and quantitative determination of gallic acid.HPLC:Sunfire-ODS C18 column(250 mm,4.6 mm),column temperature was 30 ℃,a mixture of 3 volumes of acetonitrile and 97 volumes of 0.1% phosphoric acid which contained 0.1% TEA was as the mobile phase,the detection wavelength was 273 nm,the number of theoretical plates of gallic acid peak should be no less than 3 000.Results:The spot in TLC of the test sample was similar in position and colour to those of the reference substance and control medicinal substances,and negative control had non-interference.For HPLC,the standard line was Y=4×107X+6 532(R2=0.999 8),the range was 0.015 7～0.283 0 μg,the precision and stability in 12 h were good(RSD=0.05%,0.65%),and the average recovery was 98.07%(RSD=0.76%).The average contents of gallic acid of 9 batches was 8.8 mg/g.Conclusion:TLC and HPLC method can be used for the qualitative determination and the quantitative control of gallic acid in Zhi Tuo Jie Bai Wan.