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

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5μm),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10μL。试验结果表明,吲哚美辛在5~200μg/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。

A method for the determination of Indomethacine in traditional Chinese medicine by HPLC was developed.The ODS-C18(150 mm×4.6 mm,5μm)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 10μL.The linear range was 5~200μg/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.