复方感冒颗粒特征图谱与黄芩苷含量测定方法研究

目的:建立复方感冒颗粒的特征图谱与黄芩苷的含量测定方法。方法:利用HPLC法测定复方感冒颗粒的特征图谱,采用Agilent TC C_(18)(4.6 mm×250 mm,5μm)色谱柱,以乙腈(A)-0.2%磷酸(B)溶液为流动相,梯度洗脱(0分钟,10%A;10分钟,14%A;25分钟,18%A;45分钟,25%A;55分钟,28%A;65分钟,42%A),流速1.0 mL/min,检测波长:266 nm,柱温:25℃。采用HPLC使用ODS-2HYPERSIL(4.6 mm×250 mm,5μm)色谱柱,以甲醇-0.1%磷酸水(43∶57)为流动相,检测波长280 nm,流速1.0 mL/min,测定黄芩苷的含量。结果:建立了以黄芩苷为参照峰的复方感冒颗粒HPLC特征图谱,共11个特征峰,并指认了葛根素、黄芩苷、汉黄芩素、黄芩素4个特征峰;含量测定中黄芩苷在0.046 36~0.463 6μg范围内线性关系良好,r=0.999 8,平均回收率为100.59%,RSD为1.18%,n=6。结论:该方法操作简单,重现性良好,能有效控制复方感冒颗粒的质量。

Study on Specific Chromatogram of Compound Cold Granules and the Assay Method of Baicalin Content

Objective:To establish specific chromatogram of compound cold granules and the assay method of baicalin content. Methods:HPLC method was used to determine the specific chromatogram of compound cold gran-ules, and Agilent TC C18 (4.6 mm×250 mm, 5μm) chromatography column was used. Acetonitrile (A)-0.2%phos-phoric acid (B) solution was used as the mobile phase and gradient elution (0 minute, 10%A;10 minutes, 14%A;25 minutes, 18%A;45 minutes, 25%A;55 minutes, 28%A;65 minutes, 42%A), with a flow rate of 1.0 mL/min, and wavelength:266 mn, column temperature:25℃ as well. ODS-2HYPERSIL (4.6 mm × 250 mm, 5 m) chromatogra-phy column was used in HPLC method to determine the content of baicalin in the mobile phase of methanol-0.1%phosphoric acid water (43:57) with a wavelength of 280 nm and a flow rate of 1.0 mL/min. Results:The HPLC specific chromatogram of compound cold granules was established with baicalin as the reference peak and 11 characteristic peaks in total. Puerarin, Baicalin, Wogonin and Baicalein, were identified as four characteristic peaks;The content of baicalin was in the range of 0.04636 to 0.4636μg, and the linear relationship was good, r=0.9998. Moreover, the average recovery rate was 100.59%, and RSD was 1.18%, n=6. Conclusion:This method is simple and reproducible, and can effectively control the quality of compound cold granules.