鸡肉组织中硝基咪唑类药物及代谢物多残留检测高效液相色谱法研究

Simultaneous Determination of Seven Nitroimidazole Residues in Chicken by HPLC

建立了鸡肉组织中甲硝唑、洛达硝唑、地美硝唑、替硝唑、塞克硝唑、奥硝唑6种硝基咪唑类药物及地美硝唑代谢产物1-甲基-5-硝基-2-羟甲基咪唑（HMMNI）共7种组分残留检测的高效液相色谱法（HPLC）。样品采用乙酸乙酯提取，SCX柱净化；色谱条件：色谱柱为Eclipse Plus C18柱（4．6mm×150mm，3．5μm）；流动相为水-乙腈-甲醇，梯度洗脱；柱温为35℃；流速为0．8mL／min，紫外检测波长为320nm，外标法定量。结果表明：7种组分在5～60ng／mL范围内，呈良好线性关系，相关系数R^2均大于0．998；方法检出限为1μg／kg；添加浓度分别为2、3、5μg／kg时，平均回收率为66．6％～101％，批内和批间RSD均小于20％。

An HPLC method was established for determination of seven nitroimidazole residues in chicken, including metronidazole, ronidazole, tinidazole, secnidazole, ornidazole, dimetridazole and 2 - hydroxymethyl - 1 - methyl- 5 -nitroimidazole （HMMNI）. The sample was extracted with ethyl acetate, and then was purified by strong cation exchange（SCX） solid phase extraction cartridge; HPLC conditions： the chromatography column was Eclipse Plus C18 column of 4.6 mm × 150 mm, 3.5 μm; mobile phase was water - acetonitrile - methanol; column temperature was 35 ℃ ; flow rate was 0.8 mL/min; detection, wavelength was 320 nm. The calibration curve was good linear between the peak areas and concentrations of nitroimidazole from 5 to 60 ng/mL with the correlation coefficient R^2 〉 0. 998. The limit of detection was 1 μg/kg. The average recoveries from spiked chicken at the three concentrations of 2, 3 and 5 μg/kg ranged from 66.6% -101%, and intra- day and inter- day （n = 5 ） batch variation coefficients were less than 20%.