液相色谱-串联质谱法检测鸡肉中7种糖皮质激素残留量

Determination of Glucocorticoids Residues in Chicken Tissues by Liquid Chromatography-Tandem Mass Spectrometry

建立鸡肉中糖皮质激素多残留的液相色谱-串联质谱分析方法。样品经乙酸乙酯提取,正己烷净化,10%乙腈水定容后供高效液相色谱-串联质谱仪（LC-MS/MS）分析,采用C18色谱柱分离,电喷雾离子化负离子方式（ESI-）及多反应监测模式（MRM）进行测定,外标法定量。研究了仪器条件、提取溶剂、净化溶剂等条件对七种目标物分离状况的影响。在优化条件下,该方法在鸡肉样品中泼尼松的的线性范围为0.5-20μg/L,泼尼松龙、甲基泼尼松、地塞米松、氢化可的松、倍氯米松、氢化可的松乙酸盐的浓度范围为0.1-20μg/L,在加标水平1.0-10μg/kg范围内,回收率为83%-104.2%;相对标准偏差为0.92%-4.89%。

A method of simultaneous detecting seven glucocorticoids residues in chicken tissues by liquid chromatographytandem mass spectrometry was developed. The samples were extracted with ethyl acetate. And then the supernatants were purified using n-hexane prior to the LC-MS/MS analysis. The analytes were separated by C18 column,indentified by negative electrospray ionization（ESI-）and multiple reaction monitoring（MRM）mode. The external standard calibration curves were used for quantitative analysis. The influences of instrument condition,extraction solvent and cleaning solvent were studied in detail. Under optimum condition,the method showed a good linearity in the range of 0.5μg/L-20μg/L for prednisone while the other targets were 0.1μg/L-20μg/L,the recoveries in chicken meat were 83%-104.2%in the standard addition levels from 1.0 μg/kg to 10 μg/kg,the relative standard deviation（RSD）of the method was beteen 0.92% and 4.89%.