百药煎质量标准研究

Study on the Quality Standard of Baiyaojian

目的建立百药煎的质量标准。方法以没食子酸对照品、五倍子对照药材为对照进行百药煎的薄层鉴别;参照2015年版《中国药典》附录的相关方法测定水分、总灰分、黄曲霉毒素、微生物限度;采用高效液相色谱法(HPLC)测定没食子酸的含量。结果百药煎薄层色谱分离度好,斑点清晰;根据18批百药煎样品测定结果,暂定其水分不得超过10.0%,总灰分不得超过3.0%,黄曲霉毒素、微生物限度应符合规定;没食子酸进样量在4.45~178.04μg/mL(r=1)时峰面积与进样量呈良好的线性关系,精密度,重复性,稳定性试验RSD均小于3%,加样回收率为99.0%,RSD为0.8%,根据含量测定结果暂定没食子酸含量不得低于30.0%。结论所建方法操作简单,合理可行,可用于百药煎的质量评价。

Objective To establish quality standards for Baiyaojian.Methods Using gallic acid reference substance and Chinese gallnut reference medicinal materials as controls for thin-layer identification of Baiyaojian.Refer to the relevant methods in the appendix of the 2015 edition of the Chinese Pharmacopoeia to determine moisture,total ash,aflatoxin,and microbial limits.High performance liquid chromatography(HPLC)was used to determine the content of gallic acid.Results Baiyaojian has good TLC resolution and clear spots.According to the test results of 18 batches of Baiyao decoction samples,it is tentatively determined that the moisture content should not exceed 10.0%,the total ash content should not exceed 3.0%,and the limits of aflatoxin and microorganisms should meet the regulations.When the injection volume of gallic acid is 4.45~178.04μg/mL(r=1),the peak area has a good linear relationship with the injection volume.The precision,repeatability,and stability test RSD are all less than 3%,and the sample recovery rate is 99.0%,RSD is 0.8%.According to the content determination result,the content of gallic acid shall not be less than 30.0%.Conclusion The established method is simple,reasonable and feasible,and can be used for the quality evaluation of Baiyaojian.