HPLC-PDA法测定17种兽药中非法添加多西环素

Determination of Doxycycline in veterinary drug by HPLC-PDA

关键词:  多西环素  峰纯度检查  高效液相色谱法

Key words:  doxycycline  peak purity test  HPLC-PDA

摘要:

建立了17种兽药中非法添加多西环素的HPLC-PDA法。采用十八烷基键合硅胶为填充剂,以醋酸盐缓冲液-乙腈(80 :20)为流动相,二极管阵列检测器进行全波长(200～400nm)扫描,检测波长为280nm,并通过液相色谱保留时间、紫外光谱信息和峰纯度检查,对非法添加物质进行定性鉴别和定量测定。结果表明,该色谱条件下,多西环素与其他物质峰分离良好。多西环素在5~500μg/mL浓度范围内线性良好,回收率在86.5%-118.1%之间,RSD为0.2%-4.5% ,检测限为0.5mg/g 。本方法准确、可靠、重现性好,可用于兽药制剂中多西环素的定性和定量检测。

Abstract:

A method for the determination of Doxycycline in 17 kinds of veterinary drug was developed by the high performance liquid chromatography with photo-diode array detector (HPLC-PDA). It was tested with C18 column, using acetate buffer solution - acetonitrile (80: 20) as the mobile phase. The detection wavelength was set at 280 nm and simultaneously collected the spectrum at wavelength of 200～400nm. After separated by HPLC． The ultraviolet spectra inforrnation, retention time and peak purity test were used to identify and determinate the Doxycycline by comparison with those of reference substances．Results showed that Doxycycline and other materials finely separated. And Doxycycline showed good linearity in the concentration range of detection. The average recoveries of the drugs ranged from 86.5%～118.1% at spiked levels with RSD less than 4.5%. the detection limit of Doxycycline was 0.5mg/g. In conclusion, the method is accurate and reproducible, and provides a reliable way for detecting doxycycline adulterated in veterinary drug.