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.
作者
张浩然
徐汀
张亦菲
田恺
华贤辉
商军
ZHANG Hao-ran;XU Ting;ZHANG Yi-fei;TIAN Kai;HUA Xian-hui;SHANG Jun(Shanghai Institute for Veterinary Drugs and Feeds Control,Shanghai201103,China)
出处
《中国兽药杂志》
2020年第6期49-55,共7页
Chinese Journal of Veterinary Drug
关键词
高效液相色谱法
非法添加
吲哚美辛
中兽药
HPLC
ilndomethacine
illegal addition
oral suspension
traditional Chinese medicine