畜禽排泄物中金霉素残留的测定方法

Determination of Chlortetracycline Residues in Excrement of Livestock and Poultry by HPLC

建立了猪粪便、猪尿液和鸡排泄物中金霉素残留的提取和色谱分析方法。先用提取液（丙酮＋水＋4mol／L盐酸，体积比为13：6：1）处理畜禽排泄物样品，提取样品中的金霉素，再用高效液相色谱仪检测其中的金霉素含量，色谱条件：流动相为0．01mol／L乙二酸＋甲醇＋已腈（体积比为10：2：3），固定相为ZORBAX SB—C18检测器波长为375nm。结果表明：在上述色谱条件下，0．2～10．0μg/ml金霉素标准溶液的金霉素峰面积与其质量浓度呈线性相关关系（R^2=0．9999）；当金霉素添加浓度为0．5～5．0mg／kg时，添加回收率为79．60％～92.78％，变异系数为3．88％～10．20％；该方法的检测限为0．5mg/kg。

A HPLC method was developed for determination of chlortetracycline（CTC） residues in the excrement of livestock and poultry. The CTC was extracted from the sample excrement with the extraction solution ： the mixture of acetone, water and hydrochloride（ 13： 6： 1 ,volume ratio）. HPLC analysis was performed on a ZORBAXSB-C18 column as stationary phase with the mixture of ethane diaeid （0. 01 mol/L） , methanol and acetonitrile （ 10：2 ： 3, volume ratio） as mobile phase. The wavelength of the detector for CTC was set at 375 nm. Peak area of CTC in standard sample detected by HPLC exhibited a linear correlation with CTC concentration （R2 = 0. 999 9）. The recovery rates of CTC from CTC fortified （0. 5 - 5.0 mg/kg） samples ranged from 79.60% to 92.78% ,with eoefficients of variance ranging from 3.88% to 10. 20%. The detection limit for CTC using HPLC in the experiment was less than 0. 5 mg/kg.