| 摘要: |
| 建立了猪、鸡组织中左旋咪唑残留检测的高效液相色谱法。组织试样在碱性条件下先用乙酸乙酯提取，然后用0.1 mol/L盐酸反萃取，萃取的样液用混合型阳离子固相萃取小柱净化，采用C18（5μm，250×4.6 mm i.d.）色谱柱，用高效液相色谱仪（带紫外检测器）在220 nm波长处测定，外标法定量。在此条件下，左旋咪唑的保留时间为12-14min。左旋咪唑浓度在10-1000μg/L时，与峰面积呈良好的线性关系，线性方程为y=196.37x+81.599（r=0.9999）。结果表明，左旋咪唑在在猪、鸡的肌肉、脂肪和肾脏中的检测限为2 µg/kg，定量限为5 µg/kg，在猪、鸡的肝脏中的检测限为2 µg/kg，定量限为10 µg/kg。在添加不同浓度水平测定下，平均回收率在70%～110%之间，批内变异系数在10%以内，批间变异系数在15%以内。 |
| 关键词: 左旋咪唑 残留 高效液相色谱 |
| DOI： |
| 投稿时间：2010-03-10修订日期：2010-04-22 |
| 基金项目: |
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| Study on Levamisole Residues in Pig and Chicken Tissues by HPLC Method |
| zengyong |
| (Hubei Institute of Veterinary Drug Control) |
| Abstract: |
| High-performance liquid chromatography method was optimised and validated for the determination of levamisole in pig and chicken tissues. A liquid-liquid extraction procedure in alkaline medium, using ethyl acetate as extraction solvent. The ethyl acetate extracts were re-extracted with 0.1mol/L HCl, then the solution was followed by a solid-phase extractaction procedure using an MCX column to clean up, The reconstituted sample was transferred to HPLC system to detect, using the C18 column（5μm，250×4.6 mm i.d.）. Retention time of levamisole was 12-14min. Linearity of the detector response was verified with robenidine standard solution in the range of 10~1000μg/L, the linear regression was y=196.37x+81.599 (r=0.9999). The quantitative methed indicated that, the LOD was 2μg/kg and the LOQ was 5μg/kg in Pigs, chicken muscle, fat and kidney, the LOD was 2μg/kg and the LOQ was 10μg/kg in Pigs, chicken liver .Recoveries of robenidine from spiked samples at different concentrations was between 70%~110%, the RSD for intra- and inter-day data were below 10% and 15%, respectively. |
| Key words: Levamisole Residue HPLC |
