HPLC同时测定清肺抑火片中14种成分的含量

Simultaneous Determination of 14 Components in Qingfei Yihuo Tablets by HPLC

关键词:  清肺抑火片  高效液相色谱法-二极管阵列检测器  含量测定  质量控制

Key words:  Qingfei Yihuo tablets  HPLC-DAD  content determination  quality control

摘要:

目的 建立 HPLC 同时测定清肺抑火片中栀子苷、芒果苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、白花前胡甲素、大黄酚、大黄素甲醚、白花前胡乙素14种成分含量的方法。方法 采用Titank C₁₈(250 mm×4.6 mm，5 μm)色谱柱；以0.1%磷酸溶液(A)-乙腈(B)为流动相，梯度洗脱；检测波长：栀子苷为238 nm，芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚、芒果苷为254 nm，盐酸小檗碱为265 nm，黄芩苷、汉黄芩苷、黄芩素、汉黄芩素为280 nm，白花前胡甲素、白花前胡乙素为321 nm；流速为1.0 mL·min^-1； 柱温为35 ℃； 进样量为10 μL。结果 栀子苷、芒果苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、白花前胡甲素、大黄酚、大黄素甲醚、白花前胡乙素的线性范围分别为4.96~223.17，0.84~42.22，18.76~938.16，4.46~223.17，4.86~243.10，1.59~79.32，0.76~38.17，1.03~51.49，1.59~79.40，1.21~60.72，1.80~90.06，0.91~45.48，1.04~51.83，0.86~43.23 μg·mL^-1，r均≥ 0.999 9。仪器精密度、稳定性、重复性试验的RSD均<2%，平均加样回收率(n=6)均>90%，RSD<3%。结论 该方法操作简单，重复性好，可为完善清肺抑火片的质量标准提供科学依据。

Abstract:

OBJECTIVE To establish a high-performance liquid chromatography method for the simultaneous determination of 14 components including geniposide, mangiferin, baicalin, berberine hydrochloride, wogonoside, baicalein, aloe-emodin, rhein, wogonin, emodin, praeruptorin A, chrysophanol, physcion and praeruptorin B in Qingfei Yihuo tablets. METHODS Titank C₁₈ (250 mm×4.6 mm, 5 μm) column was used; 0.1% phosphoric acid solution(A)-acetonitrile(B) was used as the mobile phase with gradient elution; detection wavelengths: geniposide at 238 nm, aloe-emodin, rhein, emodin, chrysophanol, physcion and mangiferin at 254 nm, berberine hydrochloride at 265 nm, baicalin, wogonoside, baicalein, and wogonin at 280 nm, praeruptorin A and praeruptorin B at 321 nm. The flow rate was 1.0 mL·min^-1 and the column temperature was 35 ℃; the injection volume was 10 μL. RESULTS The linear ranges of geniposide, mangiferin, baicalin, berberine hydrochloride, wogonoside, baicalein,aloe-emodin, rhein, wogonin, emodin, praeruptorin A, chrysophanol, physcion and, praeruptorin B were 4.96-223.17, 0.84-42.22, 18.76-938.16, 4.46-223.17, 4.86-243.10, 1.59-79.32, 0.76-38.17, 1.03-51.49, 1.59-79.40, 1.21-60.72, 1.80-90.06, 0.91-45.48, 1.04-51.83 and 0.86-43.23 μg·mL^-1, with r all ≥ 0.999 9. The RSDs of instrument precision, stability and reproducibility tests were <3%, and the average recoveries in sample(n=6) were >90%, with the RSDs <3%. CONCLUSION The method is simple and reproducible and can provide a scientific basis for improving the quality standard of Qingfei Yihuo tablets.