高效液相色谱法同时测定清肺抑火片中8个成分的含量

目的：建立高效液相色谱法同时测定清肺抑火片中栀子苷、黄芩苷、小檗碱、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚8个有效成分的含量。方法：采用Eclipse Plus C₁₈色谱柱（250 mm×4.6 mm，5 μm），以乙腈-0.1%磷酸水溶液为流动相，梯度洗脱，流速1 mL·min^-1，检测波长254 nm，柱温30℃。结果： 8个有效成分的线性范围：栀子苷，4.782~95.648 μg·mL^-1（r=0.999 3）；黄芩苷，1.449~28.988μg·mL^-1（r=0.999 4）；盐酸小檗碱，1.625~32.498 μg·mL^-1（r=0.999 7）；芦荟大黄素，0.982~19.650μg·mL^-1（r=1.00 0）；大黄酸，0.703~14.070 μg·mL^-1（r=1.00 0）；大黄素，0.535~10.710 μg·mL^-1（r=1.000）；大黄酚，0.945~18.900 μg·mL^-1（r=1.000）；大黄素甲醚，1.505~30.100 μg·mL^-1（r=1.000）。平均加样回收率（n=3）在98.8%~100.4%之间，RSD均在0.24%~1.3%。8个成分的含量分别为栀子苷，0.610~0.916mg·g^-1；黄芩苷，0.249~0.374 mg·g^-1；小檗碱（按盐酸小檗碱计），0.043~0.065 mg·g^-1；芦荟大黄素，0.088~0.132 mg·g^-1；大黄酸，0.147~0.221 mg·g^-1；大黄素，0.089~0.133 mg·g^-1；大黄酚，0.193~0.290mg·g^-1；大黄素甲醚，0.046~0.070 mg·g^-1。结论：该方法可用于清肺抑火片中主要8个有效成分的含量测定。

Objective: To develop an HPLC method for simultaneous determination of gardenoside,berberine, baicalin, aloe-modin, rhein, emodin, chrysophanol and physcion in Qingfei Yihuo tablets.Methods: An Eclipse Plus C₁₈ column(250 mm×4.6 mm, 5 μm)was used. The mobile phase,consisting of solvent A(acetonitrile) and solvent B(0.1% phosphoric acid), was programmed as a gradient. The flow rate was 1.0 ml·min^-1 and the detection wavelength was 254 nm. The column temperature was 30℃.Results: The linearity was achieved in the range of 4.782-95.648 μg·mL^-1(r=0.999 3)for gardenoside,1.449-28.988 μg(r=0.999 4)for baicalin, 1.625-32.498 μg·mL^-1(r=0.999 7)for berberine hydrochloride, 0.982-19.650 μg·mL^-1(r=1.000)for aloe-modin, 0.703-14.070 μg·mL^-1(r=1.000)for rhein, 0.535-10.710 μg·mL^-1(r=1.000)for emodin, 0.945-18.900μg·mL^-1 (r=1.000)for chrysophanol and 1.505-30.100 μg·mL^-1(r=1.000)for physcion respectively. The average recoveries(n=3)were 98.8%-100.4% with RSD of 0.24%-1.3%. The contents in 3 samples were in the ranges of 0.610-0.916 mg·g^-1 for gardenoside, 0.249-0.374 mg·g^-1 for baicalin, 0.043-0.065 mg·g^-1 for berberine(calculated by berberine hydrochloride),0.088-0.132 mg·g^-1 for aloe-modin,0.147-0.221 mg·g^-1 for rhein,0.089-0.133 mg·g^-1 for emodin,0.193-0.290 mg·g^-1 for chrysophanol,0.046-0.070 mg·g^-1 for physcion respectively. Conclusion: The developed method can be used for the determination of the above mentioned eight bioactive Qingfei Yihuo tablets.

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