固相萃取-气相色谱-质谱分析肉样中盐酸克伦特罗的残留量

Determination of Clenbuterol in Meat Sample by Coupling Solid Phase Extraction with Gas Chromatography-Mass Spectrometry

建立了固相萃取 气相色谱 质谱联机分析肉样中盐酸克伦特罗残留量的方法。对盐酸克伦特罗在C1 8和离子交换固相萃取柱上的保留行为进行了研究 ,发现不同浓度盐酸克伦特罗的固相萃取回收率在 75 %～ 95 %之间 ;肉样中的加标回收率在 70 %～ 83 % ;相对标准偏差在 4 .95 %～ 1 3 .4 % ;最低检出限为 1 μg kg。盐酸克伦特罗的硅烷化产物 ,采用选择离子的模式进行检测 ( 86、2 4 3、2 62、2 77) ,衍生物的峰面积与样品浓度在0 .0 0 2 5 2～ 2 .0 2mg L范围内呈良好的线性关系 ,线性回归系数大于 0 .9999。

Solid phase extraction and gas chromatography-mass spectrometric method have been developed for the determination of the residues of clenbuterol in meat sample. The retention behaviors of clenbuterol on C-18 and ion exchange column were investigated. It has been found that the recoveries of different quantities of clenbuterol on the column are between 75% similar to 95%. The average recoveries of clenbuterol in meat sample are 70% similar to 83%; the relative standard deviations are 4.95% similar to 13.4% and the detection limit is 1 mug/kg for meat samples. The selected ion mode (SIM) detection method (ions selected: 86, 243, 262, 277) was used for the detection of the clenbuterol derivatives. There is a good linear correlation(the calibration coefficient is above 0.9999) between the peak areas and concentration of clenbuterol in the range of 0.00252 mg/L to 2.02 mg/L.