高效液相色谱法测定牛组织中三氯苯唑及其代谢物残留量的研究

Study on Detection Method Triclabendazole and Metabolite Residues in Cattle Tissues by HPLC

关键词:  高效液相色谱法  三氯苯唑及代谢物  残留  牛组织

Key words:  HPLC  triclabendazole and metabolite  residues  cattle tissues

摘要:

建立一种可同时检测牛组织中三氯苯唑及代谢物三氯苯唑酮药物残留的高效液相色谱—紫外检测法。牛组织样品经乙腈提取，异辛烷去脂肪，PPL柱净化。以0.02 mol/L乙酸铵溶液和乙腈溶液为流动相，流速为1.0 mL/min，检测波长296 nm。结果表明三氯苯唑、三氯苯唑酮在20-1200 ng/mL呈良好的线性关系，R2均大于0.999。方法的最低定量限为50 μg/kg。三氯苯唑、三氯苯唑酮在50~600 μg/kg的浓度添加水平上，其回收率在60~100%，批内、批间的相对标准偏差小于20%。

Abstract:

A method for determination of Triclabendazole and metabolite ketotriclabendazole in cattle tissues with HPLC by UV detection was established. Triclabendazole and ketotriclabendazole were extracted from cattle tissues with acetonitrile and degreased in isooctane, dissolved with 30 % acidified alcohol after evaporation, then the solution was purified with PPL column. The mobile phase were 0.02 mol/L ammonium acetate and acetonitrile, the flow rate was 1.0mL/min and detection wavelengths was 296 nm. A good linearity of the calibration curve was obtained with the range of 20-1200 ng/mL （R2>0.999），and the limit of quantification of Triclabendazole and ketotriclabendazole was 50 μg/kg. The average recoveries of Triclabendazole and ketotriclabendazole from spiked cattle tissues at the three concentrations of 50、300、600 μg/kg (liver and kindey) ; 50、200、400 μg/kg（muscle）and 50、100、200 μg/kg (fat) ranged from 60-100%(n=5) respectively. In day-between days batch variation coefficients were both less than 20%.