波长切换HPLC法同时测定水蛭蛴螬化瘀片中10个活性成分的含量

Objective: To establish a method of simultaneous determination of sodium Danshensu, salvianolic acid B, baicalein, wogonin, baicalin, wogonoside, isorhamnetin-3-O-neohespeidoside, ammonium glycyrrhizinate, tetrahydropalmatine and paeoniflorin in Shuizhi Qicao Huayu tablets by HPLC with wavelength switching. Methods: SHIMADZU Insertsustain C₁₈ column(250 mm×4.6 mm, 5 μm)was chosen, and gradient elution was conducted with 0.2% acetic acid-methanol-acetonitrile as the mobile phase. The detection wavelength was set at 280 nm(0-20 min, 33-36 min, 38.8-42 min for salvianic acid A sodium, tetrahydropalmatine, and baicalin), at 230 nm(20-29 min for paeoniflorin), at 254 nm(29-33 min for isorhamnetin-3-Oneohespeidoside), at 252 nm(62-70 min for ammonium glycyrrhizinate), at 286 nm(36-38.8 min for salvianolic acid B), at 274 nm(42-48 min, 70-80 min for wogonin and wogonoside)and at 276 nm(48- 62 min for baicalein). The flow rate was 1.0 mL·min^-1 and the column temperature was 25℃. Results: The linear ranges of sodium Danshensu, salvianolic acid B, baicalein, wogonin, baicalin, wogonoside, isorhamnetin-3- O-neohespeidoside, monoammonium glycyrrhizinate, tetrahydropalmatine and paeoniflorin were 6.32-158 μg·mL^-1 (r=0.999 8), 53.4-1 336 μg·mL^-1(r=0.999 9), 1.51-37.8 μg·mL^-1(r=0.999 9), 0.888-22.2 μg·mL^-1 (r=0.999 9), 18.6-465 μg·mL^-1(r=1.000 0), 7.92-198 μg·mL^-1(r=0.999 9), 2.14-53.6 μg·mL^-1(r=0.999 8), 3.30-82.6 μg·mL^-1(r=1.000 0), 1.12-28.0 μg·mL^-1(r=0.999 9)and 38.5-962 μg·mL^-1(r=0.999 9), respectively. The average recoveries(n=6)were 97.0%(RSD=1.6%), 99.1%(RSD=1.4%), 99.0% (RSD=1.4%), 98.1%(RSD=1.6%), 99.2%(RSD=0.98%), 100.2%(RSD=1.8%), 98.7%(RSD=2.6%), 100.4%(RSD=1.7%), 100.2%(RSD=3.0%)and 100.5%(RSD=2.2%), respectively. The content ranges of three batches of pilot samples were 2.112-2.119 mg·g^-1, 15.642-15.648 mg·g^-1, 1.558-1.568 mg·g^-1, 0.553- 0.568 mg·g^-1, 16.515-16.527 mg·g^-1, 4.412-4.423 mg·g^-1, 0.554-0.569 mg·g^-1, 3.353-3.368 mg·g^-1, 0.192-0.201 mg·g^-1 and 8.749-8.761 mg·g^-1, respectively. Conclusion: The method could be used for the quality control of Shuizhi Qicao Huayu tablets, and offered basis for the establishment of the standard.