建立了同时测定动物性食品中克伦特罗、沙丁胺醇、莱克多巴胺和特布他林 4 种 β2-受体激动剂残留的高效液相色谱-串联质谱( HPLC-MS/MS)的分析方法.样品采用质量分数为5%的三氯乙酸振荡提取,用HLB与ProE-lut PXC固相萃取柱串联净化,采用 HPLC-MS/MS在多反应监测( MRM)模式下检测,内标法定量.结果表明:克伦特罗、沙丁胺醇、莱克多巴胺和特布他林的检出限( S/N=3)分别为 0. 05、0. 05、0. 05 和 0. 2 μg/kg,定量限( S/N=10)分别为0. 25、0. 25、0. 1和0. 5 μg/kg.空白基质加标水平为 2. 5、5、10 μg/kg时,4 种 β2-受体激动剂的平均回收率为90. 3%~120. 5%,相对标准偏差为 1. 60%~9. 33%.该方法采用酸解法提取样品,较酶解法耗时短,速度快,灵敏度高,回收率、重现性好,可有效用于动物性食品中4种 β2-受体激动剂残留的快速检测.
An analytical method was developed to simultaneously determine the residues of four β2-agonists in animal foods by high performance liquid chromatography/electrospray-tandem mass spectrometry( HPLC-MS/MS). Samples were extracted with 5%( mass fraction) trichloracetic acid,and then cleaned up by two solid phase extraction cartridges( HLB and ProElut PXC). Quantification of the four β2-agonists was achieved by HPLC-MS/MS in multiple reaction monitoring(MRM)using internal standard method. The limits of detection(S/N=3) of clenbuterol,salbutamol,ractopamine and terbutaline were 0. 05,0. 05,0. 05 and 0. 2 μg/kg, and the limits of quantification( S/N=10)were 0. 25,0. 25,0. 1 and 0. 5 μg/kg,respectively. The average recoveries of the four β2-agonists spiked in blank samples at the spiked levels of 2. 5,5 and 10 μg/kg were 90. 3%-120. 5% with the relative standard deviation( RSD)range of 1. 60%-9. 33%. The method is reliable,sensitive,good recovery and repeatability. It is suitable for the determination of the residues of the four β2-agonists in animal foods.
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