清热解毒类中兽药中非法添加吲哚美辛的HPLC-PDA检测方法的建立

Determination of Indomethacine Illegally Added in Traditional Chinese Medicine by HPLC - PDA

关键词:  高效液相色谱法  非法添加  吲哚美辛  中兽药

Key words:  HPLC  Indomethacine  illegal addition  Oral suspension  Traditional Chinese Medicine

摘要:

建立了HPLC-PDA法测定清热解毒类中兽药中吲哚美辛的检测方法。采用ODSC₁₈色谱柱(柱长150 mm,内径4.6 mm,粒径5 μm),流动相为乙腈：0.1 mol/L冰醋酸(50∶50,V₁∶V₂)为流动相,采集波长范围为200 ~ 400 nm,定量波长为317 nm, 进样量为10 μL。试验结果表明,吲哚美辛在5～200 μg/mL 范围内线性良好(r=0.9999),各基质中吲哚美辛的检测限均为1.0 g/kg,峰纯度检查和光谱相似度检查均符合要求。其中,板二黄片中吲哚美辛的平均回收率为96.5%,相对标准偏差(RSD)为0.9% (n=6)；三黄散中吲哚美辛的平均回收率为99.3%,RSD为1.3% (n=6)；扶正解毒散中吲哚美辛的平均回收率为100.6%,RSD为0.8% (n=6)。本法应用清热解毒类中兽药中非法添加吲哚美辛的检测,结果准确可靠。

Abstract:

A method for the determination of Indomethacine in traditional Chinese medicine by HPLC was developed. The ODS -C₁₈ (150 mm×4.6 mm, 5 μm) was used as the column, with the scanning wavelength set from 200 nm ~ 400 nm. The detection wavelength was 317 nm. An isocratic elution method using acetonitrile : 0.1 mol/L acetic acid (50∶50,V₁∶V₂) as mobile phase was developed, and the injection volume was 10 μL. The linear range was 5~200 μg/mL (r=0.9999). The mean recovery of Indomethacine in Ban’er Huang tablets was 96.5%, and the relative standard deviation (RSD) was 0.9% (n=6). The mean recovery of Indomethacine in Sanhuang powder was 99.3%, and the RSD was 1.3% (n=6). The mean recovery of Indomethacine in Fuzheng Jiedu powder was 100.6%, and the RSD was 0.8% (n=6). The limit of detection was 1.0 g/kg. The peak purity test and spectra matching test were applied. The method is reliable for the determination of Indomethacine illegally added in traditional Chinese medicine.