高效液相色谱法测定脂肪中11种苯并咪唑类药物残留标志物

建立了同时测定脂肪中11种苯并咪唑类药物残留标志物的高效液相色谱法。样品采用正己烷溶解后,加入抗氧化剂,用0.1mol/L盐酸-乙腈(1∶1,体积比)提取,经正己烷脱脂后再次加入抗氧化剂,以MCX固相萃取柱净化。净化液浓缩处理后进行高效液相色谱分离,以甲醇-1%乙酸为流动相梯度洗脱,流速为1.0mL/min,紫外检测波长为292nm,采用外标法以峰面积定量检测。11种目标物均在25.0~1000μg/L范围内线性良好,方法定量下限为50μg/kg,在3个加标水平下的回收率为82.0%~109%,相对标准偏差(RSD)为0.71%~9.9%。该方法能够满足脂肪中苯并咪唑类药物残留标志物的检测要求。

Determination of 11 Benzimidazoles Metabolites Residues in Fat by High Performance Liquid Chromatography

A high performance liquid chromatographic method was developed for the simultaneous determination of11 benzimidazoles metabolites residues in fat.Samples were firstly dissolved with n -hexane,then extracted with antioxidant and 0.1 mol/L hydrochloric acid-acetonitrile (1 ∶1,by volume ),followed by treatments with n -hexane for defatting,antioxidant again and further clean-up on a MCX solid phase extraction (SPE ) column.After concentration,the chromatographic separation was performed on an Atlantis T3 column by gradient elution with a mixed solution of methanol and1 % acetic acid at a flow rate of1.0 mL/min.The detection wavelength was set at292 nm,and the external standard method was used for quantitation.The calibration curves for11 analytes were linear in the range of25.0-1 000 μg/L with quantitation limits of 50 μg/kg.The recoveries at three spiked levels ranged from 82.0 % to109 % with relative standard deviations (RSD ) of 0.71 %-9.9 %.The developed method could meet the requirements for determination of11 benzimidazoles metabolites residues in fat.