复方肝舒丸的质量标准研究

Quality standard for Ganshu Pills

目的：建立复方肝舒丸的质量标准.方法：采用薄层色谱法对丸剂中的丹参、大黄、当归、白术进行定性鉴别.采用高效液相色谱（HPLC）法测定丸剂所含丹参酮ⅡA的量,色谱柱为Welchrom-C18柱（5μm,250 mm×4.6mm）,流动相为甲醇-水（体积比80∶20）,流速1.0 m L·min^-1,柱温30℃,检测波长为270 nm.采用HPLC法测定大黄素、大黄酚的含量,色谱柱为Welchrom-C18柱（5μm,250 mm×4.6 mm）,流动相为甲醇-0.1%磷酸溶液（体积比90∶10）,柱温25℃,流速1.0 m L·min^-1,检测波长为254 nm.结果：薄层斑点清晰,阴性对照无干扰,专属性强.丹参酮ⅡA在0.02~0.2μg范围内线性关系良好（r=0.9999）,平均加样回收率为99.26%,RSD为0.66%（n=9）.大黄酚在0.2~2.0μg范围内线性关系良好（r=0.9999）,平均加样回收率为99.21%、RSD为0.72%（n=9）.大黄素在0.2~2.0μg范围内线性关系良好（r=0.9999）,平均加样回收率为99.21%,RSD分别0.61%（n=9）.结论：本方法操作简单、灵敏度高、结果准确、重现性好、专属性强,可作为复方肝舒丸的质量控制标准.

Objective： To establish a quality standard of Ganshu Pills. Methods： Radix et Rhizoma Salviae Miltiorrhizae,Radix et Rhizoma Rhei,Radix Angelicae Slinensis,Rhizoma Atractylodis Macrocephalae in Pills are distinguished by TLC. The content of tanshinone IIA was determined by HPLC. The analysis was performed on a Welchrom-C18（ 5μm,250 mm × 4. 6 mm） column with the mobile phase of methanol-water（ volume ratio 80∶ 20）,at the flow rate of 1. 0 m L·min^-1,the Column temperature was 30℃,and the detection wavelength was 270 nm. The content of chrysophanol and emodin were determined by HPLC. The analysis was performed on a Welchrom-C18（ 5 μm,250 mm × 4. 6 mm） column with the mobile phase of methanol- 0. 1% phosphoric acid solution（ volume ratio 90∶ 10）,at the flow rate of 1. 0m L·min^-1,the Column temperature was 25℃,and detection wavelength was 254 nm. Results： The TLC spots were clear,without interference of negative control strong specificity. The linear range of tanshinone IIA was 0. 02 ~ 0. 2 μg（ r = 0. 9999）,the average recovery rate was 99. 26%,RSD was 0. 66%（ n = 9）. The linear range of emodin was 0. 2 ~ 2. 0 μg（ r =0. 9999）,the average recovery rate was 99. 21%,RSD was 0. 61%（ n = 9）. The linear range of chrysophanol was 0. 2 ~2. 0 μg（ r = 0. 9999）,the average recovery rate was 99. 21%,RSD was 0. 72%（ n = 9）. Conclusion： This method has advantages of simple operation,high sensitivity,accurate results,good reproducibility,specificity can be used as the quality control standard of Ganshu Pills.