多波长HPLC法测定唇齿清胃丸中4种药效成分的含量

Simultaneous determination of 4 kinds of active ingredients in Chunchi Qingwei pills by multi-wavelength HPLC

目的建立一种适用于唇齿清胃丸中栀子苷、黄芩苷、盐酸小檗碱和大黄素含量分析的高效液相色谱的方法。方法 Zorbax Eclipse XDB-C18键合硅胶柱（4.6 mm×150 mm,5μm）;乙腈-0.2%磷酸水溶液为流动相,梯度洗脱;柱温25℃;流速1.0 ml/min;检测波长为240、275和350 nm。结果栀子苷、黄芩苷、盐酸小檗碱和大黄素进样量分别在0.056~0.3360（r=0.9998）、0.208~1.248（r=0.9990）、0.116~0.696（r=0.9989）和0.040~0.240μg（r=0.9993）范围内线性关系良好,平均加样回收率分别为97.52%、98.28%、97.51%和95.04%,RSD分别为1.56%、0.70%、1.40%和0.56%。结论该法简便、快速、灵敏、精密度高、重现性良好,结果准确,适合唇齿清胃丸中栀子苷、黄芩苷、盐酸小檗碱和大黄素含量分析。

Objective To develop an HPLC method for simultaneous determination of jasminoidin,baicalin,berberine hydrochloride and emodin in Chunchi Qingwei（CCQW）pills. Methods The analysis was performed on a Zorbax Eclipse XDB-C18（4.6mm × 150 mm,5 μm）with gradient elution by using the mobile phase of acetonitride- 0.2% phosphoric acid solution. The column temperature was maintained at 25 ℃ and the flow rate was 1.0 ml/min. The detection wavelengths were set at 240 nm,275 nm and 350 nm,respectively. Results The calibration curves were linear within the range of 0.056-0.3360 μg（r=0.9998）for jasminoidin,0.208-1.248 μg（r=0.9990）for baicalin,0.116- 0.696 μg（r=0.9989）for berberine hydrochloride,and 0.040~0.240 μg（r=0.9993）for emodin,respectively. The recoveries were 97.52 %（RSD=1.56 %）、98.28 %（RSD=0.70 %）、97.51 %（RSD=1.40 %）and 95.04 %（RSD=0.56 %）,respectively. Conclusion The method is convenient,fast,sensitive and reproducible,with good precision,specificity,and accuracy. So it can be used for simultaneous determination of jasminoidin,baicalin,berberine hydrochloride and emodin in CCQW pills.