氟苯尼考注射液中非法添加多西环素检查方法的建立

To establish a method for testing of doxycycline in Florfenicol Injection

关键词:  高效液相色谱法  氟苯尼考注射液  多西环素

Key words:  HPLC  Florfenicol Injection  doxycycline

摘要:

为打击兽药非法添加,本研究采用高效液相色谱法对氟苯尼考注射液中非法添加多西环素的检查方法进行了研究。色谱柱为C₁₈(4.6 mm×150 mm,5 μm),流动相为醋酸盐缓冲液[0.25 mol/L醋酸铵溶液-0.1 mol/L乙二胺四醋酸二钠-三乙胺(100：10：1),调节pH值至8.8]-乙腈(85：15),二极管阵列检测器,波长采集范围为200 nm～400 nm,记录269 nm波长处的色谱图,流速1 mL/min,进样量10 μL。多西环素进样浓度在0.015～0.96 mg/mL范围内与峰面积呈良好的线性关系(r＝1.0000)；样品平均回收率为99.4%(n＝9),RSD为0.3%。本方法简便、准确、可行,适用于氟苯尼考注射液中非法添加多西环素的检测。

Abstract:

Inorder to crack down illegal adulterated in veterinary, An HPLC method for testing of doxycycline in Florfenicol Injection was developed. The isolation was performed on a C₁₈ column(4.6 mm×150 mm,5 μm) with mobile phase consisting of acetate buffer[0.25 mol/L ammonium acetate solution - 0.1 mol/L disodium Edetate solution - triethylamine(100：10：1), adjust pH to 8.8] - acetonitrile (85:15) . Dioda array detector wavelength range was 200 nm～400 nm,The detection wavelength was 269 nm, The flow rate was 1 mL/min , The injection volume was 10 μL .There was a good linear correlation between the peak areas and the concentrations of doxycycline at the range of 0.015～0.96 mg/mL(r＝1.0000)by HPLC. The average recovery was 99.4% with RSD of 0.3%(n=9).The results indicated that the method was simple,accurate and repeatable .It can be used for testing of doxycycline in Florfenicol Injection.