高效薄层条带快速净化检测猪肉中瘦肉精的残留

Rapid detection of clenbuterol residues in pork with high performance thin layer clean-up technique

目的本实验利用薄层净化与气质联用仪相结合技术,建立了快速检测动物组织中残留瘦肉精的方法。方法通过优化薄层展开程序,获得瘦肉精在自制的纸基薄层板上稳定的比移值(Rf)。样品经过提取、浓缩后,在纸基薄层板上进行净化,通过裁切目标区,以甲醇洗脱,洗脱液经衍生剂反应后,用气质联用仪,在SIM模式下检测定量。结果在优化条件方法下,样品中的杂质得到完全分离。在浓度范围为0.02μg/ml^0.5μg/ml时,线性关系良好,线性回归方程为y=358 971x+18 441,r=0.999 2;加标回收率为71.3%~84.7%(外标法),最低检出限为2.0μg/kg(基于3倍信噪比)。结论本方法操作快速方便、灵敏准确,能满足猪肉样品中瘦肉精的快速分析要求。不仅节约了前处理时间,更有效地降低了溶剂消耗,表现出环境友好等特点。纸基薄层色谱条带有望在农产品样品前处理领域获得良好应用。

Objective To establish a method to rapidly detect clenbuterol residues in pork tissues with high performance thin layer clean- up technology and gas chromatography mass spectrometry（ GC- MS）. Methods Throughout optimization of solvent development procedures,the stable Rf value has been obtained on the surface of paper- based thin layer chromatography slides. The sample was extracted and concentrated for purification on paper- based thin layer. Consequently,the target zone was cut with methanol for elution,and the elution solution,after derivation,was detected by GC- MS instrument under SIM mode. Results In this optimized method,the impurities in the sample were completely separated. And when the concentrations were within 0. 02 μg / ml- 0. 5 μg / ml,good linearity was obtained; linear regression equation was y = 358 971 x ＋ 18 441,r = 0. 999 2,with the recovery rates within 71. 3%- 84. 7%,and the minimum detection limit as 2. 0 μg / kg. Conclusion The method is fast and convenient,sensitive and accurate,and can meet the requirement of rapid analysis of clenbuterol in pork samples. The method not only saves the pre- treatment time,but also more effectively reduces the solvent consumption,showing the characteristics of environmental friendliness. Thus,current constructed paper- based thin layer chromatography slides is expected to be applied in the sample pretreatment field of agricultural product.