HPLC法测定中兽药散剂中非法添加土霉素的方法研究

Study on Determination Methos of Oxytetracycline Added Illegally in Veterinary Chinese Materia Medica Powders by HPLC

关键词:  中兽药散剂  土霉素  HPLC  检测

Key words:  veterinary Chinese materia medica powders  oxytetracycline  HPLC  determination

摘要:

建立了高效液相色谱法检测清肺散、白头翁散、止痢散等中兽药散剂中非法添加土霉素的方法。用十八烷基硅烷键合硅胶色谱柱，以0.05mol/L草酸铵溶液-二甲基甲酰胺-0.2mol/L磷酸氢二铵（75:20:5）（用氨试液调pH值至8.0?0.2）为流动相，检测波长280 nm，流速1.0 mL/min，进样量20μL，柱温：35℃。结果显示，土霉素的线性范围为100～300μg/ml，线性方程为Y = 4.90?10X – 2.39?10(上标)3，（r = 0.9996，n=5），本方法的回收率为80.68%～119.23%，RSD为0.66%～1.85%。结果表明，本方法准确、可靠，适用于中兽药散剂中非法添加土霉素的检测。

Abstract:

An HPLC method was established for effective detection on oxytetracycline added illegally in veterinary Chinese materia medica powders as Qingfei San, Baitouweng San, and Zhili San, etc. A reverse-phase C18 column was used, the mobile phase was 0.05 mol/L ammonium oxalate solution -DMF-0.2 mol/L ammonium dibasic phosphate (75:20:5) (adjusted the pH value with ammoniac solution to 8.0?0.2), the determination wave length was 280 nm, the flow rate was 1.0 mL/min and the column worked at 35 ℃. The result demonstrated that the linearity range of oxytetracycline was 100～300 μg/mL, the linear equation is Y = 4.90?10X – 2.39?10(上标)3(r= 0.9996，n=5), the recovery was 80.68%～119.23%, RSD was 0.66%～1.85%. It indicated that this method was accurate, reliable, and suitable in the determination of oxytetracycline added illegally in veterinary Chinese materia medica powders.