HPLC法测定复方奥硝唑大黄口腔膜中的大黄酸、大黄素及大黄酚的含量

目的建立反相高效液相色谱法(RP-HPLC)测定复方奥硝唑大黄口腔膜中大黄酸、大黄素及大黄酚的含量。方法使用Fortis Xi C18色谱柱(250 mm×4.6 mm,5μm),甲醇-质量分数为0.1%的磷酸溶液(体积比为85∶15)为流动相,流速为1.0 mL.min-1,检测波长为254 nm。结果大黄酸、大黄素、大黄酚峰与相邻色谱峰分离度均高于3.0,方法专属性强;各组分在测定范围内线性关系良好,回归方程分别为:大黄酚A大黄酚=3.298 3×107ρ-602 4(R2=0.999 0),大黄酸A大黄酸=2.138 3×107ρ-576 2(R2=0.997 0),大黄素A大黄素=2.075 0×107ρ-489 1(R2=0.9990);各组分加样回收率均高于94.0%。测得复方奥硝唑大黄口腔膜中大黄酸、大黄素、大黄酚的平均含量为353、106、121μg.cm-2。结论本方法测定奥硝唑大黄口腔膜中大黄酸、大黄素及大黄酚,可应用于奥硝唑大黄口腔缓释膜剂的质量控制。

Determination of rhein, emodin and rhubarb in compound Ornidazole Rhubarb oral membrane by HPLC

Objective To establish a reversed phase high performance liquid (RP-HPLC) to determine rhein, emodin and rhubarb in compound ornidazole rhubarb oral membrane. Methods Methanol -0.1%(φ) phosphoric acid (V:V=85:15) solution were used as mobile phase. The Parameters are as follows: velocity was set to 1.0 mL·min^-1, and detection wavelength was set at 254 nm. Results Rhein, emodin, rhubarb and adjacent compounds chromatographic peak separation degrees were all higher than 3.0; In terms of RBP peak, theory plate number was higher than 2000. The linear regression equation of rhubarb phenol was A_{rhubarb phenol} = 3.298 3×10⁷ρ-602 4,R² =0.999 0; The linear regression equation of rhein was A_rhein= 2.138 3×10⁷ρ-576 2,R² =0.997 0; The linear regression equation of emodin was A_emodin=2.075 0×10⁷ρ-489 1,R² =0.999 0; RBP absorption degree presented a good linear relationship. The recovery rates were higher than 94%, and the specificity is strong. According to the regression equation calculating concentration, the contents of rhein, emodin, rhubarb in compound ornidazole oral membrane of phenol averaged at 353 μg·cm^-2, 106 μg·cm^-2 and 121 μg·cm^-2 respectively. Conclusion The research indicated that the analysis method for determination of rhein, emodin and rhubarb in ornidazole rhubarb membrane can achieved completely baseline separation, and had high linear regression coefficient (r² = 0.999 0). Specificity was strong and sample recovery rate was high, so it can be effectively applied in quality control for ornidazole rhubarb oral slow-release formulation preparation.