氟苯尼考注射液中非法添加多西环素检查方法的建立

Establishment of Detection Methods for Doxycycline in Florfenicol Injection

为建立氟苯尼考注射液中非法添加多西环素高效液相检查方法,研究使用C18（4.6 mm×150 mm,5μm）色谱柱,以醋酸盐缓冲液[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p H值至8.8]-乙腈（85∶15）为流动相,采用二极管阵列检测器,波长采集范围为200~400 nm,记录色谱图波长为269 nm,流速为1 m L/min,进样量为10μL。结果表明,多西环素进样浓度在0.015~0.96 mg/m L范围内与峰面积呈良好的线性关系（r=1.0000）;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。

A detection method of doxycycline illegally adulterated in florfenicol injection was established by HPLC. 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 p H to 8. 8]-acetonitrile（ 85 ∶ 15）. Photodiode array detector wavelength range was200 ~ 400 nm,The recorded wavelength was 269 nm,The flow rate was 1 m L / min,The injection volume was10 μL. The results showed that there was a good linear correlation between the peak areas and the concentrations of doxycycline at the range of 0. 015 ~ 0. 96 mg / m L（ r = 1. 0000）. The average recovery was 99. 4% with RSD of0. 3%（ n = 9）. This method was simple,accurate and feasible. It was suitable for detection of doxycycline illegally adulterated in florfenicol injection.